Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global # *** Added by check_cif _publ_requested_journal ' JCS, Dalton Trans.' _journal_coden_Cambridge 186 _publ_contact_author_name ' Hiroaki Nishikawa' _ publ_contact_author_address ; Hiroaki Nishikawa, Department of Chemistry, Faculty of Science, Kanazawa University, Kakuma-machi, Kanazawa 920-1192, Japan ; _ publ_contact_author_email nisikawa@cacheibm.s.kanazawa-u.ac.jp _publ_contact_author_fax ' 076-264-5742 (Japan) ' _publ_contact_author_phone ' 076-264-5703 (Japan ' _publ_contact_letter ; ? ; loop_ _publ_author_name 'Fujinami, Shuhei' 'Jalil, M. Abdul' 'Nishikawa, Hiroaki' data_for_complex_1_[(P-N)PdPhI] _database_code_CSD 154050 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C17 H26 I N2 P Pd ' _chemical_formula_moiety 'C17 H26 I N2 P Pd ' _chemical_formula_weight 522.68 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,z _cell_length_a 17.516(1) _cell_length_b 14.429(1) _cell_length_c 7.988(1) _cell_angle_alpha 89 _cell_angle_beta 89 _cell_angle_gamma 90 _cell_volume 2018.8(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.5 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.528 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.505 _exptl_absorpt_correction_T_max 0.603 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 2667 _diffrn_reflns_av_R_equivalents 0.161 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9992 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.63 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2483 _reflns_number_gt 1906 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0813 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1906 _refine_ls_number_parameters 200 _refine_ls_goodness_of_fit_ref 0.870 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.07200(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0146 _refine_diff_density_max 0.36 _refine_diff_density_min -0.33 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0013(6) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.69028(3) 0.34137(4) 1.144(4) 0.0655(2) Uani 1.00 d . . . Pd1 Pd 0.55957(3) 0.28360(3) 1.011(4) 0.0419(1) Uani 1.00 d . . . P1 P 0.44598(10) 0.2293(1) 0.927(4) 0.0441(5) Uani 1.00 d . . . N1 N 0.4910(3) 0.3749(4) 1.155(4) 0.044(1) Uani 1.00 d . . . N2 N 0.3835(4) 0.4469(5) 1.215(4) 0.056(2) Uani 1.00 d . . . C1 C 0.5056(5) 0.4425(6) 1.272(4) 0.060(2) Uani 1.00 d . . . C2 C 0.4405(5) 0.4871(7) 1.308(4) 0.068(3) Uani 1.00 d . . . C3 C 0.3035(5) 0.4735(9) 1.211(4) 0.084(3) Uani 1.00 d . . . C4 C 0.4163(4) 0.3784(5) 1.124(4) 0.044(2) Uani 1.00 d . . . C5 C 0.3770(4) 0.3175(5) 1.005(4) 0.051(2) Uani 1.00 d . . . C6 C 0.4171(5) 0.1236(6) 1.039(4) 0.062(2) Uani 1.00 d . . . C7 C 0.4303(7) 0.1355(9) 1.225(4) 0.080(3) Uani 1.00 d . . . C8 C 0.4585(6) 0.0389(6) 0.969(4) 0.083(4) Uani 1.00 d . . . C9 C 0.4220(5) 0.2133(7) 0.706(4) 0.063(2) Uani 1.00 d . . . C10 C 0.4289(8) 0.3046(10) 0.614(4) 0.086(3) Uani 1.00 d . . . C11 C 0.3426(6) 0.1712(9) 0.680(4) 0.083(4) Uani 1.00 d . . . C12 C 0.6169(5) 0.2007(5) 0.854(4) 0.051(2) Uani 1.00 d . . . C13 C 0.6285(5) 0.2260(6) 0.687(4) 0.064(2) Uani 1.00 d . . . C14 C 0.6725(7) 0.1718(8) 0.582(4) 0.083(3) Uani 1.00 d . . . C15 C 0.7080(6) 0.0924(8) 0.642(4) 0.084(3) Uani 1.00 d . . . C16 C 0.6973(5) 0.0683(7) 0.803(4) 0.075(3) Uani 1.00 d . . . C17 C 0.6525(5) 0.1194(6) 0.911(4) 0.060(2) Uani 1.00 d . . . H1 H 0.5541 0.4554 1.3144 0.0725 Uiso 1.00 calc . . . H2 H 0.4349 0.5372 1.3793 0.0819 Uiso 1.00 calc . . . H3 H 0.2955 0.5237 1.2813 0.1017 Uiso 1.00 calc . . . H4 H 0.2905 0.4928 1.0956 0.1017 Uiso 1.00 calc . . . H5 H 0.2729 0.4227 1.2376 0.1017 Uiso 1.00 calc . . . H6 H 0.3580 0.3530 0.9089 0.0611 Uiso 1.00 calc . . . H7 H 0.3356 0.2875 1.0547 0.0611 Uiso 1.00 calc . . . H8 H 0.3640 0.1149 1.0160 0.0745 Uiso 1.00 calc . . . H9 H 0.4138 0.0815 1.2769 0.0961 Uiso 1.00 calc . . . H10 H 0.4831 0.1454 1.2399 0.0961 Uiso 1.00 calc . . . H11 H 0.4020 0.1876 1.2584 0.0961 Uiso 1.00 calc . . . H12 H 0.4414 -0.0150 1.0213 0.0997 Uiso 1.00 calc . . . H13 H 0.4480 0.0331 0.8482 0.0997 Uiso 1.00 calc . . . H14 H 0.5119 0.0460 0.9806 0.0997 Uiso 1.00 calc . . . H15 H 0.4583 0.1719 0.6544 0.0753 Uiso 1.00 calc . . . H16 H 0.4781 0.3302 0.6278 0.1034 Uiso 1.00 calc . . . H17 H 0.4219 0.2945 0.4923 0.1034 Uiso 1.00 calc . . . H18 H 0.3911 0.3463 0.6485 0.1034 Uiso 1.00 calc . . . H19 H 0.3048 0.2126 0.7165 0.0999 Uiso 1.00 calc . . . H20 H 0.3342 0.1609 0.5589 0.0999 Uiso 1.00 calc . . . H21 H 0.3392 0.1140 0.7333 0.0999 Uiso 1.00 calc . . . H22 H 0.6062 0.2813 0.6409 0.0771 Uiso 1.00 calc . . . H23 H 0.6779 0.1891 0.4629 0.0998 Uiso 1.00 calc . . . H24 H 0.7393 0.0561 0.5650 0.1010 Uiso 1.00 calc . . . H25 H 0.7215 0.0137 0.8383 0.0908 Uiso 1.00 calc . . . H26 H 0.6458 0.0996 1.0186 0.0724 Uiso 1.00 calc . . . 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 I1 0.0408(3) 0.0648(3) 0.0910(5) -0.0070(2) -0.0103(3) -0.0087(4) Pd1 0.0340(2) 0.0370(2) 0.0547(3) -0.0024(2) 0.0025(3) -0.0019(3) P1 0.0337(8) 0.0418(9) 0.057(1) -0.0033(7) 0.0021(8) -0.0090(9) N1 0.043(2) 0.038(3) 0.051(3) -0.002(2) 0.001(3) -0.004(2) N2 0.054(3) 0.056(4) 0.057(4) 0.013(3) 0.002(3) -0.010(3) C1 0.065(4) 0.056(5) 0.059(5) -0.007(4) -0.011(5) -0.023(4) C2 0.070(5) 0.066(6) 0.070(6) 0.002(4) -0.008(5) -0.033(5) C3 0.056(4) 0.093(7) 0.104(9) 0.028(5) 0.007(6) -0.027(7) C4 0.043(2) 0.044(3) 0.044(4) 0.002(2) 0.002(3) 0.005(3) C5 0.040(3) 0.045(3) 0.068(5) 0.004(2) 0.000(4) -0.017(4) C6 0.055(4) 0.045(3) 0.086(5) -0.005(3) 0.015(4) 0.007(3) C7 0.083(7) 0.074(7) 0.084(5) -0.005(6) 0.008(6) 0.018(6) C8 0.068(5) 0.045(4) 0.14(1) 0.000(4) 0.037(7) -0.004(6) C9 0.054(4) 0.077(5) 0.056(3) -0.020(4) 0.008(4) -0.023(4) C10 0.101(8) 0.096(6) 0.060(7) -0.012(6) 0.000(6) 0.012(6) C11 0.054(5) 0.119(9) 0.077(8) -0.032(5) -0.003(5) -0.020(7) C12 0.042(4) 0.044(3) 0.067(4) 0.001(3) 0.009(3) -0.016(3) C13 0.053(5) 0.068(5) 0.071(5) -0.002(4) 0.012(4) 0.002(4) C14 0.089(7) 0.079(6) 0.082(7) -0.003(5) 0.032(6) -0.028(5) C15 0.067(5) 0.076(5) 0.109(6) -0.003(4) 0.025(7) -0.042(6) C16 0.047(4) 0.070(6) 0.109(6) 0.010(4) 0.005(5) -0.031(5) C17 0.052(4) 0.054(4) 0.075(6) 0.008(3) -0.005(4) 0.000(4) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 PD1 2.6585(7) . . yes PD1 P1 2.241(2) . . yes PD1 N1 2.123(6) . . yes PD1 C12 2.002(7) . . yes P1 C5 1.863(7) . . yes P1 C6 1.838(9) . . yes P1 C9 1.827(10) . . yes N1 C1 1.374(9) . . yes N1 C4 1.334(9) . . yes N2 C2 1.37(1) . . yes N2 C3 1.454(10) . . yes N2 C4 1.357(9) . . yes C1 C2 1.34(1) . . yes C4 C5 1.46(1) . . yes C6 C7 1.51(2) . . yes C6 C8 1.52(1) . . yes C9 C10 1.51(2) . . yes C9 C11 1.53(1) . . yes C12 C13 1.40(1) . . yes C12 C17 1.41(1) . . yes C13 C14 1.38(1) . . yes C14 C15 1.39(2) . . yes C15 C16 1.34(2) . . yes C16 C17 1.38(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 PD1 P1 173.65(6) . 1_555 1_555 yes I1 PD1 N1 94.3(2) . 1_555 1_555 yes I1 PD1 C12 90.3(2) . 1_555 1_555 yes P1 PD1 N1 82.9(2) . 1_555 1_555 yes P1 PD1 C12 92.9(2) . 1_555 1_555 yes N1 PD1 C12 173.9(3) . 1_555 1_555 yes PD1 P1 C5 103.7(2) . 1_555 1_555 yes PD1 P1 C6 112.9(3) . 1_555 1_555 yes PD1 P1 C9 122.5(3) . 1_555 1_555 yes C5 P1 C6 103.0(4) . 1_555 1_555 yes C5 P1 C9 105.1(4) . 1_555 1_555 yes C6 P1 C9 107.5(4) . 1_555 1_555 yes PD1 N1 C1 134.8(5) . 1_555 1_555 yes PD1 N1 C4 118.5(5) . 1_555 1_555 yes C1 N1 C4 106.5(6) . 1_555 1_555 yes C2 N2 C3 127.1(8) . 1_555 1_555 yes C2 N2 C4 107.0(6) . 1_555 1_555 yes C3 N2 C4 126.0(8) . 1_555 1_555 yes N1 C1 C2 109.2(7) . 1_555 1_555 yes N2 C2 C1 107.4(7) . 1_555 1_555 yes N1 C4 N2 109.9(6) . 1_555 1_555 yes N1 C4 C5 124.1(6) . 1_555 1_555 yes N2 C4 C5 125.9(6) . 1_555 1_555 yes P1 C5 C4 108.8(5) . 1_555 1_555 yes P1 C6 C7 109.9(8) . 1_555 1_555 yes P1 C6 C8 111.0(7) . 1_555 1_555 yes C7 C6 C8 112(1) . 1_555 1_555 yes P1 C9 C10 110.0(6) . 1_555 1_555 yes P1 C9 C11 113.0(7) . 1_555 1_555 yes C10 C9 C11 110.5(9) . 1_555 1_555 yes PD1 C12 C13 120.9(6) . 1_555 1_555 yes PD1 C12 C17 121.2(7) . 1_555 1_555 yes C13 C12 C17 117.7(8) . 1_555 1_555 yes C12 C13 C14 120.8(9) . 1_555 1_555 yes C13 C14 C15 120(1) . 1_555 1_555 yes C14 C15 C16 118.6(9) . 1_555 1_555 yes C15 C16 C17 122(1) . 1_555 1_555 yes C12 C17 C16 119(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag I1 PD1 2.6585(7) . . ? C2 C10 3.60(2) . 1_556 ? #------------------------------------------------------------------------------ ############################# END ############### data_for_complex_4_[(P-N)PdMe(PPh3)](BF4) _database_code_CSD 154051 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C30 H39 B F4 N2 P2 Pd ' _chemical_formula_moiety '?' _chemical_formula_weight 682.80 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 11.6414(5) _cell_length_b 8.2299(3) _cell_length_c 33.904(1) _cell_angle_alpha 90 _cell_angle_beta 94.264(1) _cell_angle_gamma 90 _cell_volume 3239.3(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 288.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5100 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25.81 _diffrn_measured_fraction_theta_max 0.8016 _diffrn_reflns_theta_full 25.81 _diffrn_measured_fraction_theta_full 0.8016 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). 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^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4997 _reflns_number_gt 4012 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.0966 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4012 _refine_ls_number_parameters 358 _refine_ls_goodness_of_fit_ref 1.708 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00207|Fo|^2^]' _refine_ls_shift/su_max 0.0043 _refine_diff_density_max 0.89 _refine_diff_density_min -0.69 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.011(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'B' 'B' 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.19738(4) 0.97548(7) 0.35446(2) 0.0635(2) Uani 1.00 d . . . P1 P 0.0242(1) 0.8448(2) 0.34427(5) 0.0602(5) Uani 1.00 d . . . P2 P 0.3690(1) 1.1194(2) 0.36993(5) 0.0638(5) Uani 1.00 d . . . F1 F 0.797(1) 0.123(2) 0.8795(5) 0.147(5) Uiso 0.50 d P . . F2 F 0.947(1) 0.235(2) 0.9184(4) 0.129(4) Uiso 0.50 d P . . F3 F 0.772(2) 0.285(2) 0.9144(6) 0.192(6) Uiso 0.50 d P . . F4 F 0.818(1) 0.072(2) 0.9512(5) 0.151(5) Uiso 0.50 d P . . F5 F 0.885(1) 0.300(2) 0.9229(4) 0.124(4) Uiso 0.50 d P . . F6 F 0.739(1) 0.163(2) 0.9390(4) 0.132(4) Uiso 0.50 d P . . F7 F 0.904(1) 0.040(2) 0.9375(5) 0.147(5) Uiso 0.50 d P . . F8 F 0.834(1) 0.054(2) 0.8850(4) 0.112(4) Uiso 0.50 d P . . N1 N 0.1725(4) 0.9107(6) 0.4146(2) 0.065(2) Uani 1.00 d . . . N2 N 0.0683(4) 0.8308(6) 0.4614(2) 0.065(2) Uani 1.00 d . . . C1 C 0.2403(5) 0.9015(9) 0.4490(2) 0.073(2) Uani 1.00 d . . . C2 C 0.1778(6) 0.8515(9) 0.4784(2) 0.074(2) Uani 1.00 d . . . C3 C 0.0676(5) 0.8667(7) 0.4229(2) 0.060(2) Uani 1.00 d . . . C4 C -0.0312(7) 0.776(1) 0.4821(2) 0.090(3) Uani 1.00 d . . . C5 C -0.0327(5) 0.8544(8) 0.3929(2) 0.066(2) Uani 1.00 d . . . C6 C 0.0298(6) 0.6269(9) 0.3337(2) 0.075(2) Uani 1.00 d . . . C7 C 0.0637(9) 0.592(1) 0.2920(3) 0.108(3) Uani 1.00 d . . . C8 C 0.1102(8) 0.541(1) 0.3642(3) 0.093(3) Uani 1.00 d . . . C9 C -0.0879(6) 0.932(1) 0.3095(2) 0.082(2) Uani 1.00 d . . . C10 C -0.0942(9) 1.118(1) 0.3155(3) 0.124(4) Uani 1.00 d . . . C11 C -0.2044(7) 0.846(2) 0.3114(3) 0.132(4) Uani 1.00 d . . . C12 C 0.2074(6) 1.009(1) 0.2915(3) 0.087(3) Uani 1.00 d . . . C13 C 0.4355(5) 1.2386(8) 0.3325(2) 0.069(2) Uani 1.00 d . . . C14 C 0.5470(6) 1.2255(10) 0.3235(3) 0.095(3) Uani 1.00 d . . . C15 C 0.5909(8) 1.329(1) 0.2959(3) 0.112(3) Uani 1.00 d . . . C16 C 0.5264(8) 1.443(1) 0.2773(3) 0.097(3) Uani 1.00 d . . . C17 C 0.4122(8) 1.461(1) 0.2859(3) 0.094(3) Uani 1.00 d . . . C18 C 0.3670(6) 1.357(1) 0.3122(2) 0.086(3) Uani 1.00 d . . . C19 C 0.4798(6) 0.9779(9) 0.3873(3) 0.075(2) Uani 1.00 d . . . C20 C 0.5494(8) 0.9928(10) 0.4214(3) 0.097(3) Uani 1.00 d . . . C21 C 0.6301(7) 0.879(1) 0.4332(4) 0.127(4) Uani 1.00 d . . . C22 C 0.6418(8) 0.741(1) 0.4102(4) 0.119(4) Uani 1.00 d . . . C23 C 0.5734(9) 0.719(1) 0.3761(4) 0.114(4) Uani 1.00 d . . . C24 C 0.4905(7) 0.8371(10) 0.3646(3) 0.089(3) Uani 1.00 d . . . C25 C 0.3570(5) 1.2668(8) 0.4086(2) 0.063(2) Uani 1.00 d . . . C26 C 0.2533(6) 1.2862(9) 0.4263(2) 0.076(2) Uani 1.00 d . . . C27 C 0.2475(8) 1.401(1) 0.4568(3) 0.092(3) Uani 1.00 d . . . C28 C 0.3385(10) 1.4948(10) 0.4690(3) 0.100(3) Uani 1.00 d . . . C29 C 0.4410(9) 1.4791(10) 0.4510(3) 0.097(3) Uani 1.00 d . . . C30 C 0.4490(6) 1.3680(10) 0.4209(2) 0.081(2) Uani 1.00 d . . . B1 B 0.8414(8) 0.156(1) 0.9173(3) 0.078(3) Uani 1.00 d . . . H1 H 0.3201 0.9267 0.4517 0.0872 Uiso 1.00 calc . . . H2 H 0.2039 0.8343 0.5053 0.0891 Uiso 1.00 calc . . . H3 H -0.0904 0.8553 0.4794 0.1081 Uiso 1.00 calc . . . H4 H -0.0590 0.6761 0.4708 0.1081 Uiso 1.00 calc . . . H5 H -0.0086 0.7599 0.5093 0.1081 Uiso 1.00 calc . . . H6 H -0.0808 0.9471 0.3945 0.0794 Uiso 1.00 calc . . . H7 H -0.0758 0.7591 0.3975 0.0794 Uiso 1.00 calc . . . H8 H -0.0453 0.5842 0.3358 0.0902 Uiso 1.00 calc . . . H9 H 0.0618 0.4778 0.2875 0.1299 Uiso 1.00 calc . . . H10 H 0.0111 0.6440 0.2734 0.1299 Uiso 1.00 calc . . . H11 H 0.1393 0.6313 0.2892 0.1299 Uiso 1.00 calc . . . H12 H 0.0856 0.5599 0.3899 0.1117 Uiso 1.00 calc . . . H13 H 0.1091 0.4273 0.3590 0.1117 Uiso 1.00 calc . . . H14 H 0.1863 0.5809 0.3628 0.1117 Uiso 1.00 calc . . . H15 H -0.0640 0.9144 0.2836 0.0984 Uiso 1.00 calc . . . H16 H -0.0199 1.1639 0.3136 0.1492 Uiso 1.00 calc . . . H17 H -0.1464 1.1636 0.2956 0.1492 Uiso 1.00 calc . . . H18 H -0.1201 1.1405 0.3408 0.1492 Uiso 1.00 calc . . . H19 H -0.2319 0.8617 0.3368 0.1584 Uiso 1.00 calc . . . H20 H -0.2582 0.8901 0.2918 0.1584 Uiso 1.00 calc . . . H21 H -0.1953 0.7331 0.3067 0.1584 Uiso 1.00 calc . . . H22 H 0.2766 1.0649 0.2868 0.1044 Uiso 1.00 calc . . . H23 H 0.2068 0.9063 0.2788 0.1044 Uiso 1.00 calc . . . H24 H 0.1432 1.0713 0.2811 0.1044 Uiso 1.00 calc . . . H25 H 0.5952 1.1451 0.3362 0.1140 Uiso 1.00 calc . . . H26 H 0.6692 1.3187 0.2902 0.1339 Uiso 1.00 calc . . . H27 H 0.5581 1.5113 0.2583 0.1165 Uiso 1.00 calc . . . H28 H 0.3661 1.5452 0.2737 0.1134 Uiso 1.00 calc . . . H29 H 0.2876 1.3645 0.3169 0.1031 Uiso 1.00 calc . . . H30 H 0.5414 1.0859 0.4375 0.1162 Uiso 1.00 calc . . . H31 H 0.6776 0.8934 0.4569 0.1519 Uiso 1.00 calc . . . H32 H 0.6980 0.6620 0.4181 0.1430 Uiso 1.00 calc . . . H33 H 0.5819 0.6253 0.3604 0.1367 Uiso 1.00 calc . . . H34 H 0.4413 0.8212 0.3413 0.1072 Uiso 1.00 calc . . . H35 H 0.1878 1.2227 0.4179 0.0906 Uiso 1.00 calc . . . H36 H 0.1773 1.4137 0.4691 0.1100 Uiso 1.00 calc . . . H37 H 0.3325 1.5707 0.4899 0.1203 Uiso 1.00 calc . . . H38 H 0.5054 1.5446 0.4593 0.1162 Uiso 1.00 calc . . . H39 H 0.5189 1.3601 0.4082 0.0977 Uiso 1.00 calc . . . 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 0.0501(4) 0.0844(4) 0.0574(4) -0.0054(2) 0.0134(2) 0.0006(2) P1 0.0495(8) 0.078(1) 0.0542(9) -0.0007(7) 0.0104(7) 0.0009(8) P2 0.0489(9) 0.075(1) 0.069(1) -0.0025(7) 0.0160(7) -0.0008(8) N1 0.058(3) 0.076(3) 0.061(3) -0.001(3) 0.010(3) 0.008(3) N2 0.064(3) 0.075(3) 0.057(3) -0.003(3) 0.013(3) 0.001(3) C1 0.058(4) 0.098(5) 0.060(4) 0.002(3) -0.005(3) 0.002(4) C2 0.078(5) 0.081(4) 0.064(4) -0.009(3) 0.005(4) 0.007(3) C3 0.062(4) 0.066(4) 0.053(4) 0.000(3) 0.014(3) 0.000(3) C4 0.078(5) 0.128(6) 0.068(5) -0.018(4) 0.028(4) 0.000(4) C5 0.054(3) 0.084(4) 0.062(4) 0.000(3) 0.013(3) 0.002(3) C6 0.080(4) 0.081(4) 0.065(4) 0.000(4) 0.007(3) -0.010(3) C7 0.132(8) 0.121(7) 0.072(5) 0.016(6) 0.009(5) -0.021(5) C8 0.097(6) 0.088(5) 0.095(6) 0.013(4) 0.006(5) -0.008(4) C9 0.063(4) 0.123(6) 0.061(4) 0.009(4) 0.007(3) 0.002(4) C10 0.142(9) 0.136(8) 0.098(7) 0.061(7) 0.027(6) 0.030(6) C11 0.053(4) 0.22(1) 0.116(8) 0.002(6) -0.012(5) 0.052(8) C12 0.057(4) 0.126(7) 0.080(5) -0.028(4) 0.020(4) 0.002(4) C13 0.058(4) 0.083(4) 0.069(4) -0.005(3) 0.016(3) -0.007(3) C14 0.067(4) 0.092(5) 0.131(7) 0.016(4) 0.042(5) 0.024(5) C15 0.083(5) 0.109(7) 0.150(9) 0.014(5) 0.060(6) 0.036(6) C16 0.106(7) 0.101(6) 0.090(6) -0.010(5) 0.044(5) 0.003(5) C17 0.091(6) 0.101(5) 0.093(6) -0.001(4) 0.015(5) 0.023(5) C18 0.065(4) 0.108(6) 0.087(5) 0.007(4) 0.021(4) 0.021(4) C19 0.051(4) 0.080(4) 0.095(6) -0.006(3) 0.017(4) 0.002(4) C20 0.073(5) 0.089(6) 0.126(8) 0.001(4) -0.008(5) -0.007(5) C21 0.067(5) 0.115(8) 0.19(1) 0.015(5) -0.019(6) 0.031(8) C22 0.071(6) 0.079(6) 0.21(1) 0.014(5) 0.040(7) 0.037(7) C23 0.105(7) 0.069(5) 0.17(1) 0.009(5) 0.051(7) 0.004(6) C24 0.091(5) 0.075(5) 0.106(6) -0.002(4) 0.031(5) -0.008(4) C25 0.057(3) 0.067(4) 0.066(4) 0.006(3) 0.014(3) 0.008(3) C26 0.068(4) 0.080(4) 0.081(5) 0.013(3) 0.018(4) 0.011(4) C27 0.111(6) 0.082(5) 0.088(6) 0.031(5) 0.046(5) 0.012(4) C28 0.134(8) 0.084(6) 0.085(6) -0.002(5) 0.021(6) -0.012(4) C29 0.111(7) 0.085(5) 0.096(7) -0.016(4) 0.024(5) -0.016(4) C30 0.078(5) 0.096(5) 0.073(5) -0.014(4) 0.022(4) -0.007(4) B1 0.100(6) 0.064(5) 0.070(5) 0.002(4) 0.014(5) 0.002(4) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PD1 P1 2.288(2) . . yes PD1 P2 2.348(2) . . yes PD1 N1 2.149(5) . . yes PD1 C12 2.166(9) . . yes P1 C5 1.825(7) . . yes P1 C6 1.830(7) . . yes P1 C9 1.838(7) . . yes P2 C13 1.822(7) . . yes P2 C19 1.803(8) . . yes P2 C25 1.799(7) . . yes F1 F8 0.73(2) . . yes F1 B1 1.37(2) . . yes F2 F5 0.92(1) . . yes F2 B1 1.39(2) . . yes F3 F5 1.33(2) . . yes F3 F6 1.39(2) . . yes F3 B1 1.33(2) . . yes F4 F6 1.24(2) . . yes F4 F7 1.16(2) . . yes F4 B1 1.39(2) . . yes F5 B1 1.30(1) . . yes F6 B1 1.45(2) . . yes F7 B1 1.36(2) . . yes F8 B1 1.38(1) . . yes N1 C1 1.359(8) . . yes N1 C3 1.324(8) . . yes N2 C2 1.369(8) . . yes N2 C3 1.338(8) . . yes N2 C4 1.469(9) . . yes C1 C2 1.343(9) . . yes C3 C5 1.493(9) . . yes C6 C7 1.52(1) . . yes C6 C8 1.52(1) . . yes C9 C10 1.55(1) . . yes C9 C11 1.54(1) . . yes C13 C14 1.359(9) . . yes C13 C18 1.40(1) . . yes C14 C15 1.39(1) . . yes C15 C16 1.33(1) . . yes C16 C17 1.39(1) . . yes C17 C18 1.37(1) . . yes C19 C20 1.37(1) . . yes C19 C24 1.40(1) . . yes C20 C21 1.37(1) . . yes C21 C22 1.39(2) . . yes C22 C23 1.36(2) . . yes C23 C24 1.40(1) . . yes C25 C26 1.395(9) . . yes C25 C30 1.396(10) . . yes C26 C27 1.41(1) . . yes C27 C28 1.35(1) . . yes C28 C29 1.39(1) . . yes C29 C30 1.38(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 PD1 P2 174.99(6) . 1_555 1_555 yes P1 PD1 N1 81.2(1) . 1_555 1_555 yes P1 PD1 C12 91.3(2) . 1_555 1_555 yes P2 PD1 N1 94.9(1) . 1_555 1_555 yes P2 PD1 C12 92.8(2) . 1_555 1_555 yes N1 PD1 C12 171.5(2) . 1_555 1_555 yes PD1 P1 C5 102.6(2) . 1_555 1_555 yes PD1 P1 C6 116.5(2) . 1_555 1_555 yes PD1 P1 C9 119.3(3) . 1_555 1_555 yes C5 P1 C6 103.9(3) . 1_555 1_555 yes C5 P1 C9 106.0(3) . 1_555 1_555 yes C6 P1 C9 106.9(4) . 1_555 1_555 yes PD1 P2 C13 121.0(2) . 1_555 1_555 yes PD1 P2 C19 108.9(2) . 1_555 1_555 yes PD1 P2 C25 113.1(2) . 1_555 1_555 yes C13 P2 C19 104.1(3) . 1_555 1_555 yes C13 P2 C25 101.8(3) . 1_555 1_555 yes C19 P2 C25 106.9(3) . 1_555 1_555 yes F8 F1 B1 75(1) . 1_555 1_555 yes F5 F2 B1 64(1) . 1_555 1_555 yes F5 F3 F6 104(1) . 1_555 1_555 yes F5 F3 B1 58(1) . 1_555 1_555 yes F6 F3 B1 64(1) . 1_555 1_555 yes F6 F4 F7 130(1) . 1_555 1_555 yes F6 F4 B1 66(1) . 1_555 1_555 yes F7 F4 B1 63(1) . 1_555 1_555 yes F2 F5 F3 133(1) . 1_555 1_555 yes F2 F5 B1 75(1) . 1_555 1_555 yes F3 F5 B1 60(1) . 1_555 1_555 yes F3 F6 F4 113(1) . 1_555 1_555 yes F3 F6 B1 55.9(9) . 1_555 1_555 yes F4 F6 B1 61(1) . 1_555 1_555 yes F4 F7 B1 66(1) . 1_555 1_555 yes F1 F8 B1 73(1) . 1_555 1_555 yes PD1 N1 C1 135.7(4) . 1_555 1_555 yes PD1 N1 C3 117.5(4) . 1_555 1_555 yes C1 N1 C3 106.8(5) . 1_555 1_555 yes C2 N2 C3 108.7(5) . 1_555 1_555 yes C2 N2 C4 125.5(6) . 1_555 1_555 yes C3 N2 C4 125.8(6) . 1_555 1_555 yes N1 C1 C2 109.9(6) . 1_555 1_555 yes N2 C2 C1 105.3(6) . 1_555 1_555 yes N1 C3 N2 109.2(5) . 1_555 1_555 yes N1 C3 C5 124.1(5) . 1_555 1_555 yes N2 C3 C5 126.7(5) . 1_555 1_555 yes P1 C5 C3 107.5(4) . 1_555 1_555 yes P1 C6 C7 112.5(6) . 1_555 1_555 yes P1 C6 C8 110.7(5) . 1_555 1_555 yes C7 C6 C8 110.7(7) . 1_555 1_555 yes P1 C9 C10 109.9(6) . 1_555 1_555 yes P1 C9 C11 112.4(6) . 1_555 1_555 yes C10 C9 C11 113.5(8) . 1_555 1_555 yes P2 C13 C14 125.1(6) . 1_555 1_555 yes P2 C13 C18 117.2(5) . 1_555 1_555 yes C14 C13 C18 117.6(7) . 1_555 1_555 yes C13 C14 C15 120.4(7) . 1_555 1_555 yes C14 C15 C16 121.9(8) . 1_555 1_555 yes C15 C16 C17 119.6(8) . 1_555 1_555 yes C16 C17 C18 119.1(8) . 1_555 1_555 yes C13 C18 C17 121.4(7) . 1_555 1_555 yes P2 C19 C20 125.6(6) . 1_555 1_555 yes P2 C19 C24 116.5(7) . 1_555 1_555 yes C20 C19 C24 117.8(7) . 1_555 1_555 yes C19 C20 C21 122.4(9) . 1_555 1_555 yes C20 C21 C22 119(1) . 1_555 1_555 yes C21 C22 C23 120.6(9) . 1_555 1_555 yes C22 C23 C24 119.3(9) . 1_555 1_555 yes C19 C24 C23 120.5(9) . 1_555 1_555 yes P2 C25 C26 120.4(5) . 1_555 1_555 yes P2 C25 C30 121.4(5) . 1_555 1_555 yes C26 C25 C30 118.2(6) . 1_555 1_555 yes C25 C26 C27 118.8(7) . 1_555 1_555 yes C26 C27 C28 122.0(8) . 1_555 1_555 yes C27 C28 C29 119.4(8) . 1_555 1_555 yes C28 C29 C30 119.8(8) . 1_555 1_555 yes C25 C30 C29 121.6(7) . 1_555 1_555 yes F1 B1 F2 112(1) . 1_555 1_555 yes F1 B1 F3 84(1) . 1_555 1_555 yes F1 B1 F4 126(1) . 1_555 1_555 yes F1 B1 F5 115(1) . 1_555 1_555 yes F1 B1 F6 102(1) . 1_555 1_555 yes F1 B1 F7 118(1) . 1_555 1_555 yes F1 B1 F8 30.6(8) . 1_555 1_555 yes F2 B1 F3 99(1) . 1_555 1_555 yes F2 B1 F4 116(1) . 1_555 1_555 yes F2 B1 F5 39.8(7) . 1_555 1_555 yes F2 B1 F6 137(1) . 1_555 1_555 yes F2 B1 F7 82(1) . 1_555 1_555 yes F2 B1 F8 108.0(10) . 1_555 1_555 yes F3 B1 F4 107(1) . 1_555 1_555 yes F3 B1 F5 60.8(9) . 1_555 1_555 yes F3 B1 F6 59.5(9) . 1_555 1_555 yes F3 B1 F7 154(1) . 1_555 1_555 yes F3 B1 F8 115(1) . 1_555 1_555 yes F4 B1 F5 115(1) . 1_555 1_555 yes F4 B1 F6 51.6(8) . 1_555 1_555 yes F4 B1 F7 50.1(8) . 1_555 1_555 yes F4 B1 F8 110(1) . 1_555 1_555 yes F5 B1 F6 102(1) . 1_555 1_555 yes F5 B1 F7 112(1) . 1_555 1_555 yes F5 B1 F8 132(1) . 1_555 1_555 yes F6 B1 F7 101(1) . 1_555 1_555 yes F6 B1 F8 114.8(10) . 1_555 1_555 yes F7 B1 F8 88(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F1 C10 3.35(2) . 4_665 ? F1 C14 3.58(2) . 4_565 ? F1 C15 3.60(2) . 4_565 ? F2 C4 3.46(2) . 2_646 ? F2 C5 3.50(1) . 4_665 ? F2 C8 3.56(2) . 4_655 ? F2 C26 3.56(2) . 4_665 ? F2 C3 3.57(1) . 4_665 ? F3 C20 3.19(2) . 4_565 ? F3 C21 3.31(2) . 4_565 ? F4 C2 3.31(2) . 2_646 ? F4 C28 3.43(2) . 2_636 ? F4 C4 3.47(2) . 4_655 ? F4 C22 3.52(2) . 4_555 ? F4 C27 3.55(2) . 2_636 ? F5 C5 3.19(1) . 4_665 ? F5 C3 3.47(1) . 4_665 ? F5 C2 3.50(1) . 2_646 ? F5 C4 3.54(1) . 2_646 ? F6 C2 3.29(1) . 2_646 ? F6 C30 3.39(1) . 4_565 ? F6 C28 3.58(2) . 2_636 ? F7 C4 3.07(2) . 4_655 ? F7 C4 3.58(2) . 2_646 ? F8 C6 3.32(2) . 4_655 ? F8 C8 3.43(2) . 4_655 ? F8 C22 3.45(2) . 4_555 ? C1 C28 3.59(1) . 1_545 ? C2 C28 3.51(1) . 1_545 ? C8 C26 3.33(1) . 1_545 ? C22 C29 3.54(1) . 1_545 ? C28 C29 3.60(1) . 3_686 ? C29 C29 3.52(2) . 3_686 ? #------------------------------------------------------------------------------ ############################# END ############### data_for_complex_5_[(P-N)Pd(allyl)]Br _database_code_CSD 154052 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C14 H26 Br N2 P Pd ' _chemical_formula_moiety '?' _chemical_formula_weight 439.65 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21/b 21/c 21/a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2-x,-y,1/2+z -x,-y,-z 1/2-x,1/2+y,z x,1/2-y,1/2+z 1/2+x,y,1/2-z _cell_length_a 13.358(4) _cell_length_b 25.953(6) _cell_length_c 10.350(3) _cell_angle_alpha 89.99(2) _cell_angle_beta 89.99(3) _cell_angle_gamma 90.05(2) _cell_volume 3588(1) _cell_formula_units_Z 8 _cell_measurement_reflns_used 19 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.349 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.378 _exptl_absorpt_correction_T_max 0.512 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w _diffrn_reflns_number 4619 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.52 _diffrn_measured_fraction_theta_max 0.9956 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.9956 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 7.24 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). 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^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4105 _reflns_number_gt 2207 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.0762 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 2207 _refine_ls_number_parameters 173 _refine_ls_goodness_of_fit_ref 1.439 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00168|Fo|^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 1.05 _refine_diff_density_min -0.88 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0001(5) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.47032(5) 0.39016(2) 0.00297(5) 0.0429(2) Uani 1.00 d . . . Br1 Br 0.83012(9) 0.17783(5) 0.61547(10) 0.0804(4) Uani 1.00 d . . . P1 P 0.3375(2) 0.38665(8) -0.1370(2) 0.0411(5) Uani 1.00 d . . . N1 N 0.5295(5) 0.3349(2) -0.1195(5) 0.041(2) Uani 1.00 d . . . N2 N 0.5201(5) 0.2763(2) -0.2724(6) 0.043(2) Uani 1.00 d . . . C1 C 0.6211(6) 0.3082(3) -0.1234(8) 0.048(2) Uani 1.00 d . . . C2 C 0.6148(6) 0.2722(3) -0.2176(8) 0.044(2) Uani 1.00 d . . . C3 C 0.4784(7) 0.2431(4) -0.3751(8) 0.060(3) Uani 1.00 d . . . C4 C 0.4708(5) 0.3138(3) -0.2109(7) 0.036(2) Uani 1.00 d . . . C5 C 0.3662(5) 0.3285(3) -0.2356(8) 0.044(2) Uani 1.00 d . . . C6 C 0.3313(6) 0.4394(3) -0.2554(9) 0.052(2) Uani 1.00 d . . . C7 C 0.2471(7) 0.4336(3) -0.3581(9) 0.062(3) Uani 1.00 d . . . C8 C 0.4353(7) 0.4448(4) -0.3229(10) 0.066(3) Uani 1.00 d . . . C9 C 0.2090(6) 0.3768(3) -0.0765(8) 0.050(2) Uani 1.00 d . . . C10 C 0.1694(8) 0.4274(4) -0.0107(10) 0.071(3) Uani 1.00 d . . . C11 C 0.2062(8) 0.3321(4) 0.0229(9) 0.069(3) Uani 1.00 d . . . C12 C 0.4252(8) 0.4449(4) 0.144(1) 0.079(4) Uani 1.00 d . . . C13 C 0.512(1) 0.4200(8) 0.184(2) 0.183(8) Uani 1.00 d . . . C14 C 0.5916(8) 0.4026(5) 0.147(1) 0.085(4) Uani 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd1 0.0469(4) 0.0406(3) 0.0411(3) 0.0006(3) -0.0073(3) -0.0073(3) Br1 0.0789(8) 0.1069(9) 0.0553(6) -0.0223(7) -0.0140(5) 0.0045(6) P1 0.044(1) 0.0382(10) 0.042(1) 0.0028(9) -0.0044(9) -0.0077(9) N1 0.049(4) 0.043(4) 0.033(3) 0.004(3) -0.001(3) -0.001(3) N2 0.047(4) 0.038(4) 0.043(4) 0.000(3) 0.010(3) -0.003(3) C1 0.040(4) 0.048(5) 0.055(5) 0.003(4) 0.007(4) 0.013(4) C2 0.038(4) 0.041(4) 0.053(5) 0.006(4) 0.009(4) 0.004(4) C3 0.072(6) 0.055(5) 0.053(5) -0.007(5) 0.001(5) -0.025(4) C4 0.040(4) 0.034(4) 0.035(3) 0.004(3) 0.002(3) 0.000(3) C5 0.034(4) 0.047(4) 0.053(5) 0.004(4) -0.007(3) -0.015(4) C6 0.045(5) 0.046(4) 0.067(5) -0.004(4) -0.005(4) -0.002(4) C7 0.065(6) 0.054(5) 0.068(6) 0.004(5) -0.015(5) 0.018(5) C8 0.055(6) 0.076(7) 0.066(6) -0.008(5) 0.009(5) 0.012(5) C9 0.043(5) 0.052(5) 0.055(5) 0.003(4) 0.009(4) -0.009(4) C10 0.057(6) 0.078(7) 0.078(7) 0.016(5) -0.001(5) -0.041(6) C11 0.077(7) 0.072(7) 0.058(6) -0.011(6) 0.004(5) 0.011(5) C12 0.072(7) 0.098(8) 0.068(6) 0.012(6) -0.019(5) -0.053(6) C13 0.16(1) 0.25(2) 0.14(1) 0.10(2) -0.10(1) -0.17(2) C14 0.070(7) 0.122(10) 0.063(6) 0.018(7) -0.020(5) -0.054(7) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PD1 P1 2.292(2) . . yes PD1 N1 2.072(6) . . yes PD1 C12 2.129(9) . . yes PD1 C13 2.102(10) . . yes PD1 C14 2.223(10) . . yes P1 C5 1.862(8) . . yes P1 C6 1.839(9) . . yes P1 C9 1.846(8) . . yes N1 C1 1.406(10) . . yes N1 C4 1.344(9) . . yes N2 C2 1.39(1) . . yes N2 C3 1.476(10) . . yes N2 C4 1.338(9) . . yes C1 C2 1.35(1) . . yes C4 C5 1.47(1) . . yes C6 C7 1.55(1) . . yes C6 C8 1.56(1) . . yes C9 C10 1.57(1) . . yes C9 C11 1.55(1) . . yes C12 C13 1.39(2) . . yes C13 C14 1.22(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 PD1 N1 83.2(2) . 1_555 1_555 yes P1 PD1 C12 104.0(3) . 1_555 1_555 yes P1 PD1 C13 141.5(5) . 1_555 1_555 yes P1 PD1 C14 173.1(3) . 1_555 1_555 yes N1 PD1 C12 172.8(3) . 1_555 1_555 yes N1 PD1 C13 134.4(5) . 1_555 1_555 yes N1 PD1 C14 103.4(3) . 1_555 1_555 yes C12 PD1 C13 38.3(5) . 1_555 1_555 yes C12 PD1 C14 69.5(4) . 1_555 1_555 yes C13 PD1 C14 32.6(5) . 1_555 1_555 yes PD1 P1 C5 102.7(2) . 1_555 1_555 yes PD1 P1 C6 115.3(3) . 1_555 1_555 yes PD1 P1 C9 120.7(3) . 1_555 1_555 yes C5 P1 C6 104.3(4) . 1_555 1_555 yes C5 P1 C9 105.4(4) . 1_555 1_555 yes C6 P1 C9 106.6(4) . 1_555 1_555 yes PD1 N1 C1 133.7(5) . 1_555 1_555 yes PD1 N1 C4 119.3(5) . 1_555 1_555 yes C1 N1 C4 106.7(6) . 1_555 1_555 yes C2 N2 C3 126.3(7) . 1_555 1_555 yes C2 N2 C4 108.0(6) . 1_555 1_555 yes C3 N2 C4 125.6(7) . 1_555 1_555 yes N1 C1 C2 107.9(7) . 1_555 1_555 yes N2 C2 C1 107.3(7) . 1_555 1_555 yes N1 C4 N2 110.1(6) . 1_555 1_555 yes N1 C4 C5 124.8(6) . 1_555 1_555 yes N2 C4 C5 125.0(7) . 1_555 1_555 yes P1 C5 C4 108.1(5) . 1_555 1_555 yes P1 C6 C7 114.6(6) . 1_555 1_555 yes P1 C6 C8 108.9(6) . 1_555 1_555 yes C7 C6 C8 110.2(8) . 1_555 1_555 yes P1 C9 C10 110.2(6) . 1_555 1_555 yes P1 C9 C11 110.5(6) . 1_555 1_555 yes C10 C9 C11 109.3(8) . 1_555 1_555 yes PD1 C12 C13 69.8(6) . 1_555 1_555 yes PD1 C13 C12 71.9(6) . 1_555 1_555 yes PD1 C13 C14 79.2(7) . 1_555 1_555 yes C12 C13 C14 143(1) . 1_555 1_555 yes PD1 C14 C13 68.3(6) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N1 C3 3.311(10) . 7_555 ? C1 C3 3.46(1) . 7_555 ? C2 C11 3.59(1) . 2_555 ? C8 C10 3.60(1) . 8_554 ? #------------------------------------------------------------------------------ ############################# END ###############