# 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_pyrrole_Pd2_CH3CN_PF6 _database_code_depnum_ccdc_archive 'CCDC 904113' #TrackingRef 'CCDC 904113 3-H.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C12 H16 F12 N4 P2 Pd2' _chemical_formula_moiety 'C12 H16 F12 N4 P2 Pd2' _chemical_formula_weight 719.01 _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 8.0162(18) _cell_length_b 8.1741(19) _cell_length_c 15.789(4) _cell_angle_alpha 90.0000 _cell_angle_beta 90.039(4) _cell_angle_gamma 90.0000 _cell_volume 1034.6(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2786 _cell_measurement_theta_min 3.59 _cell_measurement_theta_max 27.18 _cell_measurement_temperature 123 #------------------------------------------------------------------------------ _exptl_crystal_description chip _exptl_crystal_colour yellow _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.308 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692.00 _exptl_absorpt_coefficient_mu 2.009 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 0.818 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 123 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 6961 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_theta_max 24.50 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1705 _reflns_number_gt 1556 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1360 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1705 _refine_ls_number_parameters 145 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0830P)^2^+4.2720P] where P=(Fo^2^+2Fc^2^)/3' _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 3.790 _refine_diff_density_min -0.720 _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) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.1023 0.0942 ; 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 0.52380(6) 0.62768(6) 0.45946(3) 0.0236(3) Uani 1.0 4 d . . . P1 P 0.0359(2) 1.0113(2) 0.32579(10) 0.0247(5) Uani 1.0 4 d . . . F1 F -0.0313(6) 0.8441(5) 0.3625(3) 0.0390(10) Uani 1.0 4 d . . . F2 F 0.1051(6) 1.1815(5) 0.2879(3) 0.0410(10) Uani 1.0 4 d . . . F3 F 0.1744(5) 0.9142(6) 0.2725(3) 0.0370(10) Uani 1.0 4 d . . . F4 F -0.0990(5) 1.1113(5) 0.3783(3) 0.0401(11) Uani 1.0 4 d . . . F5 F 0.1639(5) 1.0271(5) 0.4032(3) 0.0380(10) Uani 1.0 4 d . . . F6 F -0.0886(5) 0.9974(5) 0.2475(3) 0.0359(10) Uani 1.0 4 d . . . N1 N 0.2178(7) 0.4295(7) 0.4102(4) 0.0264(12) Uani 1.0 4 d . . . N2 N 0.5501(8) 0.8492(8) 0.3934(5) 0.0373(15) Uani 1.0 4 d . . . C1 C 0.2510(8) 0.5917(8) 0.4075(4) 0.0235(14) Uani 1.0 4 d . . . C2 C 0.2539(8) 0.6503(8) 0.4916(4) 0.0261(14) Uani 1.0 4 d . . . C3 C 0.2273(8) 0.5107(8) 0.5452(4) 0.0252(14) Uani 1.0 4 d . . . C4 C 0.2086(8) 0.3746(8) 0.4929(5) 0.0261(15) Uani 1.0 4 d . . . C5 C 0.5468(8) 0.9687(10) 0.3564(5) 0.0347(16) Uani 1.0 4 d . . . C6 C 0.5385(10) 1.1185(9) 0.3096(6) 0.042(2) Uani 1.0 4 d . . . H1 H 0.2691 0.6549 0.3579 0.0282 Uiso 1.0 4 calc R . . H1A H 0.2040 0.3672 0.3653 0.0316 Uiso 1.0 4 calc R . . H2 H 0.2701 0.7602 0.5093 0.0313 Uiso 1.0 4 calc R . . H3 H 0.2233 0.5110 0.6053 0.0303 Uiso 1.0 4 calc R . . H4 H 0.1926 0.2647 0.5107 0.0313 Uiso 1.0 4 calc R . . H6A H 0.4462 1.1130 0.2690 0.0504 Uiso 1.0 4 calc R . . H6B H 0.6436 1.1352 0.2791 0.0504 Uiso 1.0 4 calc R . . H6C H 0.5202 1.2099 0.3487 0.0504 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 0.0230(4) 0.0239(4) 0.0240(4) -0.00020(18) -0.0008(3) 0.00402(17) P1 0.0221(9) 0.0285(10) 0.0234(9) -0.0007(7) 0.0032(7) -0.0028(7) F1 0.042(3) 0.037(3) 0.038(3) -0.0062(19) 0.0073(19) 0.0032(18) F2 0.055(3) 0.032(3) 0.036(3) -0.009(2) -0.0001(19) 0.0035(19) F3 0.031(3) 0.048(3) 0.033(3) 0.0061(19) 0.0096(17) -0.0109(19) F4 0.033(3) 0.048(3) 0.040(3) 0.0095(18) 0.0038(19) -0.0143(18) F5 0.038(3) 0.047(3) 0.030(2) 0.0017(19) -0.0084(17) -0.0051(18) F6 0.039(3) 0.037(3) 0.032(3) 0.0003(18) -0.0091(17) -0.0030(17) N1 0.030(3) 0.030(3) 0.019(3) 0.000(3) 0.002(3) -0.007(3) N2 0.021(4) 0.045(4) 0.046(4) -0.006(3) -0.006(3) 0.009(3) C1 0.014(4) 0.033(4) 0.024(4) 0.004(3) -0.002(3) 0.003(3) C2 0.022(4) 0.028(4) 0.028(4) 0.002(3) 0.000(3) -0.003(3) C3 0.021(4) 0.032(4) 0.023(4) 0.002(3) 0.001(3) 0.001(3) C4 0.017(4) 0.025(4) 0.036(4) -0.004(3) -0.006(3) 0.008(3) C5 0.020(4) 0.038(4) 0.046(5) 0.001(3) -0.004(3) 0.009(4) C6 0.028(4) 0.044(5) 0.054(5) 0.003(4) -0.003(4) 0.017(4) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'DIRDIF99-PATTY (Gould, et al., 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _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 Pd1 2.4783(9) yes . 3_666 Pd1 N2 2.101(7) yes . . Pd1 C1 2.354(6) yes . . Pd1 C2 2.231(7) yes . . Pd1 C3 2.294(6) yes . 3_666 Pd1 C4 2.273(7) yes . 3_666 P1 F1 1.579(5) yes . . P1 F2 1.613(5) yes . . P1 F3 1.603(5) yes . . P1 F4 1.590(5) yes . . P1 F5 1.600(5) yes . . P1 F6 1.592(4) yes . . N1 C1 1.353(9) yes . . N1 C4 1.383(9) yes . . N2 C5 1.138(10) yes . . C1 C2 1.413(9) yes . . C2 C3 1.436(9) yes . . C3 C4 1.393(9) yes . . C5 C6 1.432(11) yes . . N1 H1A 0.880 no . . C1 H1 0.950 no . . C2 H2 0.950 no . . C3 H3 0.950 no . . C4 H4 0.950 no . . C6 H6A 0.980 no . . C6 H6B 0.980 no . . C6 H6C 0.980 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 Pd1 Pd1 N2 176.52(17) yes 3_666 . . Pd1 Pd1 C1 86.08(16) yes 3_666 . . Pd1 Pd1 C2 78.60(17) yes 3_666 . . Pd1 Pd1 C3 74.67(16) yes 3_666 . 3_666 Pd1 Pd1 C4 88.14(16) yes 3_666 . 3_666 N2 Pd1 C1 91.6(3) yes . . . N2 Pd1 C2 98.0(3) yes . . . N2 Pd1 C3 108.8(3) yes . . 3_666 N2 Pd1 C4 94.4(3) yes . . 3_666 C1 Pd1 C2 35.8(3) yes . . . C1 Pd1 C3 137.3(3) yes . . 3_666 C1 Pd1 C4 172.2(3) yes . . 3_666 C2 Pd1 C3 153.1(3) yes . . 3_666 C2 Pd1 C4 147.2(3) yes . . 3_666 C3 Pd1 C4 35.5(3) yes 3_666 . 3_666 F1 P1 F2 179.7(3) yes . . . F1 P1 F3 90.1(3) yes . . . F1 P1 F4 91.2(3) yes . . . F1 P1 F5 90.5(3) yes . . . F1 P1 F6 90.6(3) yes . . . F2 P1 F3 89.7(3) yes . . . F2 P1 F4 89.1(3) yes . . . F2 P1 F5 89.6(3) yes . . . F2 P1 F6 89.4(3) yes . . . F3 P1 F4 178.7(3) yes . . . F3 P1 F5 89.8(3) yes . . . F3 P1 F6 89.5(2) yes . . . F4 P1 F5 89.8(3) yes . . . F4 P1 F6 90.9(3) yes . . . F5 P1 F6 178.8(3) yes . . . C1 N1 C4 111.0(6) yes . . . Pd1 N2 C5 172.8(6) yes . . . Pd1 C1 N1 107.1(4) yes . . . Pd1 C1 C2 67.4(4) yes . . . N1 C1 C2 107.8(6) yes . . . Pd1 C2 C1 76.9(4) yes . . . Pd1 C2 C3 102.3(4) yes . . . C1 C2 C3 106.4(6) yes . . . Pd1 C3 C2 104.1(4) yes 3_666 . . Pd1 C3 C4 71.4(4) yes 3_666 . . C2 C3 C4 107.5(6) yes . . . Pd1 C4 N1 105.3(5) yes 3_666 . . Pd1 C4 C3 73.1(4) yes 3_666 . . N1 C4 C3 107.2(6) yes . . . N2 C5 C6 178.7(8) yes . . . C1 N1 H1A 124.499 no . . . C4 N1 H1A 124.509 no . . . Pd1 C1 H1 94.422 no . . . N1 C1 H1 126.104 no . . . C2 C1 H1 126.095 no . . . Pd1 C2 H2 90.706 no . . . C1 C2 H2 126.812 no . . . C3 C2 H2 126.797 no . . . Pd1 C3 H3 93.666 no 3_666 . . C2 C3 H3 126.246 no . . . C4 C3 H3 126.242 no . . . Pd1 C4 H4 91.271 no 3_666 . . N1 C4 H4 126.415 no . . . C3 C4 H4 126.412 no . . . C5 C6 H6A 109.470 no . . . C5 C6 H6B 109.469 no . . . C5 C6 H6C 109.474 no . . . H6A C6 H6B 109.464 no . . . H6A C6 H6C 109.476 no . . . H6B C6 H6C 109.474 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Pd1 Pd1 C1 N1 -26.7(4) no 3_666 . . . Pd1 Pd1 C1 C2 75.9(3) no 3_666 . . . C1 Pd1 Pd1 C1 180(326828) no . . 3_666 3_666 C1 Pd1 Pd1 C2 144.67(16) no . . 3_666 3_666 C1 Pd1 Pd1 C3 -38.50(16) no . . 3_666 . C1 Pd1 Pd1 C4 -5.16(16) no . . 3_666 . Pd1 Pd1 C2 C1 -99.2(3) no 3_666 . . . Pd1 Pd1 C2 C3 5.0(3) no 3_666 . . . C2 Pd1 Pd1 C1 -144.67(17) no . . 3_666 3_666 C2 Pd1 Pd1 C2 -180(32400) no . . 3_666 3_666 C2 Pd1 Pd1 C3 -3.17(17) no . . 3_666 . C2 Pd1 Pd1 C4 30.17(17) no . . 3_666 . Pd1 Pd1 C3 C2 -5.0(3) no 3_666 . 3_666 3_666 Pd1 Pd1 C3 C4 -109.0(3) no 3_666 . 3_666 3_666 C3 Pd1 Pd1 C1 38.50(16) no 3_666 . 3_666 3_666 C3 Pd1 Pd1 C2 3.17(16) no 3_666 . 3_666 3_666 C3 Pd1 Pd1 C3 -180(32400) no 3_666 . 3_666 . C3 Pd1 Pd1 C4 -146.66(16) no 3_666 . 3_666 . Pd1 Pd1 C4 N1 -37.9(3) no 3_666 . 3_666 3_666 Pd1 Pd1 C4 C3 65.8(3) no 3_666 . 3_666 3_666 C4 Pd1 Pd1 C1 5.16(17) no 3_666 . 3_666 3_666 C4 Pd1 Pd1 C2 -30.17(17) no 3_666 . 3_666 3_666 C4 Pd1 Pd1 C3 146.66(18) no 3_666 . 3_666 . C4 Pd1 Pd1 C4 -180(293395) no 3_666 . 3_666 . N2 Pd1 C1 N1 155.9(4) no . . . . N2 Pd1 C1 C2 -101.5(3) no . . . . N2 Pd1 C2 C1 81.6(3) no . . . . N2 Pd1 C2 C3 -174.2(4) no . . . . N2 Pd1 C3 C2 174.4(3) no . . 3_666 3_666 N2 Pd1 C3 C4 70.3(3) no . . 3_666 3_666 N2 Pd1 C4 N1 139.7(4) no . . 3_666 3_666 N2 Pd1 C4 C3 -116.6(3) no . . 3_666 3_666 C1 Pd1 C2 C1 -0.0(3) no . . . . C1 Pd1 C2 C3 104.2(5) no . . . . C2 Pd1 C1 N1 -102.6(6) no . . . . C2 Pd1 C1 C2 0.0(3) no . . . . C1 Pd1 C3 C2 -71.3(5) no . . 3_666 3_666 C1 Pd1 C3 C4 -175.3(3) no . . 3_666 3_666 C3 Pd1 C1 N1 35.6(6) no 3_666 . . . C3 Pd1 C1 C2 138.2(3) no 3_666 . . . C2 Pd1 C3 C2 -11.9(7) no . . 3_666 3_666 C2 Pd1 C3 C4 -115.9(5) no . . 3_666 3_666 C3 Pd1 C2 C1 -92.5(6) no 3_666 . . . C3 Pd1 C2 C3 11.8(7) no 3_666 . . . C2 Pd1 C4 N1 27.6(6) no . . 3_666 3_666 C2 Pd1 C4 C3 131.3(4) no . . 3_666 3_666 C4 Pd1 C2 C1 -167.3(3) no 3_666 . . . C4 Pd1 C2 C3 -63.0(6) no 3_666 . . . C3 Pd1 C4 N1 -103.7(5) no 3_666 . 3_666 3_666 C3 Pd1 C4 C3 0.0(3) no 3_666 . 3_666 3_666 C4 Pd1 C3 C2 104.1(5) no 3_666 . 3_666 3_666 C4 Pd1 C3 C4 0.0(3) no 3_666 . 3_666 3_666 C1 N1 C4 Pd1 -73.1(6) no . . . 3_666 C1 N1 C4 C3 3.5(7) no . . . . C4 N1 C1 Pd1 67.3(6) no . . . . C4 N1 C1 C2 -3.8(7) no . . . . Pd1 C1 C2 Pd1 0.000(13) no . . . . Pd1 C1 C2 C3 -99.1(4) no . . . . N1 C1 C2 Pd1 101.6(5) no . . . . N1 C1 C2 C3 2.4(7) no . . . . Pd1 C2 C3 Pd1 -5.5(4) no . . . 3_666 Pd1 C2 C3 C4 -80.0(5) no . . . . C1 C2 C3 Pd1 74.3(5) no . . . 3_666 C1 C2 C3 C4 -0.3(7) no . . . . Pd1 C3 C4 Pd1 -0.000(13) no 3_666 . . 3_666 Pd1 C3 C4 N1 -101.3(4) no 3_666 . . . C2 C3 C4 Pd1 99.4(5) no . . . 3_666 C2 C3 C4 N1 -1.9(7) 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 Pd1 F6 3.476(4) no . 2_545 F1 N2 3.392(8) no . 1_455 F1 C1 3.143(8) no . . F1 C2 3.448(8) no . . F1 C4 3.231(8) no . 3_566 F1 C5 3.534(8) no . 1_455 F1 C6 3.284(10) no . 2_545 F2 F3 2.767(6) no . 2_555 F2 N1 2.941(7) no . 1_565 F2 N2 3.409(8) no . 2_555 F2 C1 3.375(8) no . 2_555 F2 C5 3.490(9) no . 2_555 F2 C6 3.529(9) no . . F3 F2 2.767(6) no . 2_545 F3 N1 3.014(7) no . 2_555 F3 C1 3.445(8) no . . F3 C1 3.247(8) no . 2_555 F3 C5 3.295(8) no . . F3 C6 3.413(9) no . . F3 C6 3.230(9) no . 2_545 F4 N2 3.544(8) no . 1_455 F4 C2 3.091(8) no . 3_576 F4 C3 3.474(8) no . 3_576 F4 C5 3.089(8) no . 1_455 F4 C6 3.101(9) no . 1_455 F5 N1 3.320(7) no . 1_565 F5 N2 3.424(8) no . . F5 C2 3.458(8) no . . F5 C4 3.194(8) no . 1_565 F5 C5 3.193(8) no . . F5 C6 3.431(9) no . . F6 Pd1 3.476(4) no . 2_555 F6 C3 3.518(7) no . 4_464 F6 C5 3.401(8) no . 1_455 F6 C6 3.299(9) no . 1_455 F6 C6 3.250(9) no . 2_545 N1 F2 2.941(7) no . 1_545 N1 F3 3.014(7) no . 2_545 N1 F5 3.320(7) no . 1_545 N2 F1 3.392(8) no . 1_655 N2 F2 3.409(8) no . 2_545 N2 F4 3.544(8) no . 1_655 N2 F5 3.424(8) no . . C1 F1 3.143(8) no . . C1 F2 3.375(8) no . 2_545 C1 F3 3.445(8) no . . C1 F3 3.247(8) no . 2_545 C2 F1 3.448(8) no . . C2 F4 3.091(8) no . 3_576 C2 F5 3.458(8) no . . C3 F4 3.474(8) no . 3_576 C3 F6 3.518(7) no . 4_565 C4 F1 3.231(8) no . 3_566 C4 F5 3.194(8) no . 1_545 C5 F1 3.534(8) no . 1_655 C5 F2 3.490(9) no . 2_545 C5 F3 3.295(8) no . . C5 F4 3.089(8) no . 1_655 C5 F5 3.193(8) no . . C5 F6 3.401(8) no . 1_655 C6 F1 3.284(10) no . 2_555 C6 F2 3.529(9) no . . C6 F3 3.413(9) no . . C6 F3 3.230(9) no . 2_555 C6 F4 3.101(9) no . 1_655 C6 F5 3.431(9) no . . C6 F6 3.299(9) no . 1_655 C6 F6 3.250(9) no . 2_555 Pd1 H1A 3.5236 no . 3_666 Pd1 H3 3.4678 no . . N1 H2 3.1518 no . . N1 H3 3.1530 no . . N2 H1 2.8122 no . . N2 H2 2.9867 no . . N2 H3 3.4602 no . 3_666 N2 H4 2.7226 no . 3_666 N2 H6A 3.0334 no . . N2 H6B 3.0473 no . . N2 H6C 3.0409 no . . C1 H3 3.2007 no . . C1 H4 3.1653 no . . C2 H1A 3.0814 no . . C2 H4 3.2038 no . . C3 H1 3.2024 no . . C3 H1A 3.0794 no . . C4 H1 3.1673 no . . C4 H2 3.2008 no . . C5 H1 3.3958 no . . C5 H4 3.5217 no . 3_666 H1 H1A 2.4119 no . . H1 H2 2.5419 no . . H1A H4 2.4461 no . . H2 H3 2.5671 no . . H3 H4 2.5191 no . . Pd1 H6C 3.3267 no . 3_676 P1 H1 3.4974 no . . P1 H1 3.4978 no . 2_555 P1 H1A 3.2662 no . 1_565 P1 H6A 3.5097 no . . P1 H6A 3.5853 no . 2_545 P1 H6B 3.3851 no . 1_455 F1 H1 2.8628 no . . F1 H2 3.4168 no . . F1 H3 3.3249 no . 3_566 F1 H4 2.5447 no . 3_566 F1 H6A 2.8886 no . 2_545 F1 H6B 2.9533 no . 2_545 F1 H6C 3.5113 no . 2_545 F2 H1 2.5226 no . 2_555 F2 H1A 2.1030 no . 1_565 F2 H6A 2.8074 no . . F2 H6C 3.4698 no . . F3 H1 2.6233 no . . F3 H1 2.8835 no . 2_555 F3 H1A 2.4150 no . 2_555 F3 H6A 2.7186 no . . F3 H6A 2.7249 no . 2_545 F3 H6B 3.5161 no . 2_545 F3 H6C 2.9799 no . 2_545 F4 H1A 3.2124 no . 1_565 F4 H2 2.4767 no . 3_576 F4 H3 3.2544 no . 3_576 F4 H4 3.3761 no . 1_565 F4 H6B 2.5976 no . 1_455 F4 H6C 3.1916 no . 1_455 F5 H1 3.2371 no . . F5 H1A 2.8621 no . 1_565 F5 H2 2.8797 no . . F5 H4 2.5900 no . 1_565 F5 H6A 3.1802 no . . F5 H6C 3.3368 no . . F6 H1 3.3146 no . 2_555 F6 H3 2.7041 no . 4_464 F6 H6A 3.3530 no . 2_545 F6 H6B 2.4755 no . 1_455 F6 H6B 3.0230 no . 2_545 F6 H6C 2.8513 no . 2_545 N1 H3 3.5775 no . 3_566 N1 H6A 3.4602 no . 2_545 N1 H6C 3.1690 no . 1_545 C1 H6A 3.2068 no . 2_545 C2 H6C 3.3073 no . 3_676 C3 H6C 3.4811 no . 3_676 C5 H2 3.3989 no . 3_676 C6 H1A 3.4787 no . 1_565 C6 H2 3.3917 no . 3_676 H1 P1 3.4974 no . . H1 P1 3.4978 no . 2_545 H1 F1 2.8628 no . . H1 F2 2.5226 no . 2_545 H1 F3 2.6233 no . . H1 F3 2.8835 no . 2_545 H1 F5 3.2371 no . . H1 F6 3.3146 no . 2_545 H1 H6A 2.6646 no . 2_545 H1A P1 3.2662 no . 1_545 H1A F2 2.1030 no . 1_545 H1A F3 2.4150 no . 2_545 H1A F4 3.2124 no . 1_545 H1A F5 2.8621 no . 1_545 H1A C6 3.4787 no . 1_545 H1A H3 3.5969 no . 3_566 H1A H6A 3.2256 no . 1_545 H1A H6A 3.1579 no . 2_545 H1A H6C 2.8545 no . 1_545 H2 F1 3.4168 no . . H2 F4 2.4767 no . 3_576 H2 F5 2.8797 no . . H2 C5 3.3989 no . 3_676 H2 C6 3.3917 no . 3_676 H2 H6B 3.5170 no . 3_676 H2 H6C 2.8121 no . 3_676 H3 F1 3.3249 no . 3_566 H3 F4 3.2544 no . 3_576 H3 F6 2.7041 no . 4_565 H3 N1 3.5775 no . 3_566 H3 H1A 3.5969 no . 3_566 H3 H6A 3.5554 no . 4_465 H3 H6B 3.5822 no . 3_676 H3 H6B 3.0596 no . 4_465 H3 H6C 3.1560 no . 3_676 H4 F1 2.5447 no . 3_566 H4 F4 3.3761 no . 1_545 H4 F5 2.5900 no . 1_545 H6A P1 3.5097 no . . H6A P1 3.5853 no . 2_555 H6A F1 2.8886 no . 2_555 H6A F2 2.8074 no . . H6A F3 2.7186 no . . H6A F3 2.7249 no . 2_555 H6A F5 3.1802 no . . H6A F6 3.3530 no . 2_555 H6A N1 3.4602 no . 2_555 H6A C1 3.2068 no . 2_555 H6A H1 2.6646 no . 2_555 H6A H1A 3.2256 no . 1_565 H6A H1A 3.1579 no . 2_555 H6A H3 3.5554 no . 4_564 H6B P1 3.3851 no . 1_655 H6B F1 2.9533 no . 2_555 H6B F3 3.5161 no . 2_555 H6B F4 2.5976 no . 1_655 H6B F6 2.4755 no . 1_655 H6B F6 3.0230 no . 2_555 H6B H2 3.5170 no . 3_676 H6B H3 3.5822 no . 3_676 H6B H3 3.0596 no . 4_564 H6C Pd1 3.3267 no . 3_676 H6C F1 3.5113 no . 2_555 H6C F2 3.4698 no . . H6C F3 2.9799 no . 2_555 H6C F4 3.1916 no . 1_655 H6C F5 3.3368 no . . H6C F6 2.8513 no . 2_555 H6C N1 3.1690 no . 1_565 H6C C2 3.3073 no . 3_676 H6C C3 3.4811 no . 3_676 H6C H1A 2.8545 no . 1_565 H6C H2 2.8121 no . 3_676 H6C H3 3.1560 no . 3_676 #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A F2 . . 1_545 2.941(7) 0.880 2.103 158.9 no N1 H1A F3 . . 2_545 3.014(7) 0.880 2.415 125.7 no data_N-methylpyrrole_Pd2_CH3CN_ _database_code_depnum_ccdc_archive 'CCDC 904114' #TrackingRef 'CCDC 904114 3-Me.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C16 H26 F12 N6 O4 P2 Pd2' _chemical_formula_moiety 'C16 H26 F12 N6 O4 P2 Pd2' _chemical_formula_weight 869.15 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.7670(11) _cell_length_b 10.1048(13) _cell_length_c 10.6014(16) _cell_angle_alpha 111.900(5) _cell_angle_beta 109.527(5) _cell_angle_gamma 90.519(4) _cell_volume 719.03(18) _cell_formula_units_Z 1 _cell_measurement_reflns_used 2296 _cell_measurement_theta_min 3.70 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 123 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 426.00 _exptl_absorpt_coefficient_mu 1.476 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.929 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 123 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.629 _diffrn_reflns_number 4200 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_theta_max 23.60 _diffrn_reflns_theta_full 23.60 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measured_fraction_theta_full 0.980 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2107 _reflns_number_gt 1923 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0813 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2107 _refine_ls_number_parameters 196 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0443P)^2^+1.7467P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.660 _refine_diff_density_min -0.400 _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) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.1023 0.0942 ; 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) ; O O 0.0106 0.0060 ; 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 0.98168(4) 0.36631(3) 0.44825(4) 0.01774(15) Uani 1.0 2 d . . . P1 P 1.0000 0.5000 0.0000 0.0178(4) Uani 1.0 1 d . . . P2 P 0.5000 0.0000 0.5000 0.0218(4) Uani 1.0 1 d . . . F1 F 1.0834(4) 0.3769(3) 0.0513(4) 0.0401(8) Uani 1.0 2 d . . . F2 F 0.8483(4) 0.3790(3) -0.1415(3) 0.0343(7) Uani 1.0 2 d . . . F3 F 1.1341(5) 0.4839(4) -0.0871(4) 0.0528(10) Uani 1.0 2 d . . . F4 F 0.4874(5) 0.1412(3) 0.6295(3) 0.0388(8) Uani 1.0 2 d . . . F5 F 0.6741(5) 0.0828(4) 0.4994(4) 0.0484(9) Uani 1.0 2 d . . . F6 F 0.3670(5) 0.0535(4) 0.3834(4) 0.0422(8) Uani 1.0 2 d . . . O1 O 0.4840(5) -0.0287(5) -0.1473(4) 0.0382(9) Uani 1.0 2 d . . . O3 O 0.7365(6) -0.1174(5) -0.0949(5) 0.0492(11) Uani 1.0 2 d . . . N1 N 0.6288(5) 0.4824(5) 0.3670(4) 0.0215(9) Uani 1.0 2 d . . . N2 N 0.9489(5) 0.1391(5) 0.3601(5) 0.0246(9) Uani 1.0 2 d . . . N3 N 0.6548(6) -0.0147(5) -0.0967(4) 0.0255(9) Uani 1.0 2 d . . . C1 C 0.6733(6) 0.3675(5) 0.4042(5) 0.0212(10) Uani 1.0 2 d . . . C2 C 0.7680(6) 0.4223(6) 0.5557(5) 0.0226(11) Uani 1.0 2 d . . . C3 C 0.7838(6) 0.5733(5) 0.6089(5) 0.0229(11) Uani 1.0 2 d . . . C4 C 0.6998(6) 0.6083(5) 0.4883(6) 0.0219(10) Uani 1.0 2 d . . . C5 C 0.5411(7) 0.4738(7) 0.2173(6) 0.0369(13) Uani 1.0 2 d . . . C6 C 0.9197(6) 0.0176(6) 0.3144(5) 0.0228(11) Uani 1.0 2 d . . . C7 C 0.8817(8) -0.1375(5) 0.2601(6) 0.0332(13) Uani 1.0 2 d . . . C8 C 0.7593(8) 0.1312(6) -0.0353(7) 0.0407(14) Uani 1.0 2 d . . . H1 H 0.6450 0.2687 0.3391 0.0254 Uiso 1.0 2 calc R . . H2 H 0.8132 0.3671 0.6121 0.0271 Uiso 1.0 2 calc R . . H3 H 0.8406 0.6393 0.7078 0.0275 Uiso 1.0 2 calc R . . H4 H 0.6935 0.7029 0.4905 0.0263 Uiso 1.0 2 calc R . . H5A H 0.6360 0.4739 0.1754 0.0443 Uiso 1.0 2 calc R . . H5B H 0.4768 0.5571 0.2190 0.0443 Uiso 1.0 2 calc R . . H5C H 0.4521 0.3847 0.1578 0.0443 Uiso 1.0 2 calc R . . H7A H 0.8378 -0.1788 0.1533 0.0399 Uiso 1.0 2 calc R . . H7B H 0.7865 -0.1645 0.2915 0.0399 Uiso 1.0 2 calc R . . H7C H 0.9949 -0.1745 0.2988 0.0399 Uiso 1.0 2 calc R . . H8A H 0.7157 0.1757 -0.1058 0.0488 Uiso 1.0 2 calc R . . H8B H 0.8911 0.1250 -0.0142 0.0488 Uiso 1.0 2 calc R . . H8C H 0.7408 0.1900 0.0551 0.0488 Uiso 1.0 2 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 0.0132(2) 0.0135(3) 0.0262(3) 0.00323(13) 0.00885(15) 0.00609(15) P1 0.0168(9) 0.0160(9) 0.0182(9) 0.0014(7) 0.0045(7) 0.0059(7) P2 0.0233(10) 0.0193(9) 0.0248(9) 0.0058(7) 0.0107(8) 0.0095(8) F1 0.0420(18) 0.0227(16) 0.0401(18) 0.0031(13) -0.0070(14) 0.0154(14) F2 0.0343(17) 0.0226(15) 0.0286(16) -0.0049(13) -0.0050(13) 0.0065(12) F3 0.056(3) 0.050(3) 0.063(3) 0.0049(17) 0.0466(19) 0.0114(18) F4 0.055(2) 0.0287(17) 0.0318(16) 0.0182(15) 0.0186(15) 0.0083(13) F5 0.0388(19) 0.048(2) 0.061(3) -0.0054(16) 0.0254(17) 0.0181(17) F6 0.052(2) 0.047(2) 0.0323(17) 0.0281(16) 0.0155(15) 0.0204(15) O1 0.027(3) 0.051(3) 0.031(2) -0.0031(18) 0.0070(17) 0.0154(18) O3 0.052(3) 0.034(3) 0.059(3) 0.012(2) 0.011(2) 0.023(2) N1 0.0087(19) 0.028(3) 0.029(2) 0.0022(16) 0.0074(16) 0.0117(18) N2 0.013(2) 0.027(3) 0.032(3) 0.0019(17) 0.0102(17) 0.0071(19) N3 0.033(3) 0.021(3) 0.018(2) -0.0003(19) 0.0059(18) 0.0058(17) C1 0.013(3) 0.017(3) 0.036(3) 0.0031(18) 0.014(2) 0.008(2) C2 0.015(3) 0.031(3) 0.031(3) 0.009(2) 0.013(2) 0.018(3) C3 0.017(3) 0.024(3) 0.029(3) 0.003(2) 0.015(2) 0.006(2) C4 0.010(3) 0.019(3) 0.041(3) 0.0055(18) 0.015(2) 0.011(2) C5 0.024(3) 0.053(4) 0.033(3) 0.004(3) 0.002(3) 0.022(3) C6 0.016(3) 0.024(3) 0.028(3) 0.004(2) 0.009(2) 0.010(3) C7 0.041(4) 0.015(3) 0.039(3) 0.007(3) 0.016(3) 0.004(3) C8 0.043(4) 0.023(3) 0.044(4) -0.012(3) 0.008(3) 0.007(3) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'DIRDIF99-PATTY (Gould, et al., 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _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 Pd1 2.4800(6) yes . 2_766 Pd1 N2 2.107(5) yes . . Pd1 C1 2.283(5) yes . . Pd1 C2 2.275(6) yes . . Pd1 C3 2.247(6) yes . 2_766 Pd1 C4 2.321(5) yes . 2_766 P1 F1 1.595(4) yes . . P1 F1 1.595(4) yes . 2_765 P1 F2 1.600(3) yes . . P1 F2 1.600(3) yes . 2_765 P1 F3 1.581(5) yes . . P1 F3 1.581(5) yes . 2_765 P2 F4 1.600(3) yes . . P2 F4 1.600(3) yes . 2_656 P2 F5 1.587(4) yes . . P2 F5 1.587(4) yes . 2_656 P2 F6 1.595(4) yes . . P2 F6 1.595(4) yes . 2_656 O1 N3 1.237(6) yes . . O3 N3 1.225(7) yes . . N1 C1 1.372(8) yes . . N1 C4 1.367(5) yes . . N1 C5 1.471(8) yes . . N2 C6 1.127(7) yes . . N3 C8 1.471(7) yes . . C1 C2 1.403(7) yes . . C2 C3 1.404(7) yes . . C3 C4 1.404(8) yes . . C6 C7 1.442(7) yes . . C1 H1 0.950 no . . C2 H2 0.950 no . . C3 H3 0.950 no . . C4 H4 0.950 no . . C5 H5A 0.980 no . . C5 H5B 0.980 no . . C5 H5C 0.980 no . . C7 H7A 0.980 no . . C7 H7B 0.980 no . . C7 H7C 0.980 no . . C8 H8A 0.980 no . . C8 H8B 0.980 no . . C8 H8C 0.980 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 Pd1 Pd1 N2 179.67(11) yes 2_766 . . Pd1 Pd1 C1 87.10(12) yes 2_766 . . Pd1 Pd1 C2 74.94(13) yes 2_766 . . Pd1 Pd1 C3 77.49(12) yes 2_766 . 2_766 Pd1 Pd1 C4 86.81(12) yes 2_766 . 2_766 N2 Pd1 C1 92.57(16) yes . . . N2 Pd1 C2 104.78(19) yes . . . N2 Pd1 C3 102.79(18) yes . . 2_766 N2 Pd1 C4 93.52(16) yes . . 2_766 C1 Pd1 C2 35.84(17) yes . . . C1 Pd1 C3 144.0(2) yes . . 2_766 C1 Pd1 C4 173.55(15) yes . . 2_766 C2 Pd1 C3 152.40(17) yes . . 2_766 C2 Pd1 C4 139.65(16) yes . . 2_766 C3 Pd1 C4 35.7(2) yes 2_766 . 2_766 F1 P1 F1 180.0(3) yes . . 2_765 F1 P1 F2 89.39(15) yes . . . F1 P1 F2 90.61(15) yes . . 2_765 F1 P1 F3 89.9(2) yes . . . F1 P1 F3 90.1(2) yes . . 2_765 F1 P1 F2 90.61(15) yes 2_765 . . F1 P1 F2 89.39(15) yes 2_765 . 2_765 F1 P1 F3 90.1(2) yes 2_765 . . F1 P1 F3 89.9(2) yes 2_765 . 2_765 F2 P1 F2 180.0(3) yes . . 2_765 F2 P1 F3 89.69(16) yes . . . F2 P1 F3 90.31(16) yes . . 2_765 F2 P1 F3 90.31(16) yes 2_765 . . F2 P1 F3 89.69(16) yes 2_765 . 2_765 F3 P1 F3 180.0(3) yes . . 2_765 F4 P2 F4 180.0(3) yes . . 2_656 F4 P2 F5 90.22(18) yes . . . F4 P2 F5 89.78(18) yes . . 2_656 F4 P2 F6 89.93(16) yes . . . F4 P2 F6 90.07(16) yes . . 2_656 F4 P2 F5 89.78(18) yes 2_656 . . F4 P2 F5 90.22(18) yes 2_656 . 2_656 F4 P2 F6 90.07(16) yes 2_656 . . F4 P2 F6 89.93(16) yes 2_656 . 2_656 F5 P2 F5 180.0(3) yes . . 2_656 F5 P2 F6 89.8(2) yes . . . F5 P2 F6 90.2(2) yes . . 2_656 F5 P2 F6 90.2(2) yes 2_656 . . F5 P2 F6 89.8(2) yes 2_656 . 2_656 F6 P2 F6 180.0(3) yes . . 2_656 C1 N1 C4 109.6(4) yes . . . C1 N1 C5 125.4(4) yes . . . C4 N1 C5 124.5(5) yes . . . Pd1 N2 C6 175.1(5) yes . . . O1 N3 O3 121.9(5) yes . . . O1 N3 C8 117.9(5) yes . . . O3 N3 C8 120.1(5) yes . . . Pd1 C1 N1 106.4(4) yes . . . Pd1 C1 C2 71.7(3) yes . . . N1 C1 C2 107.7(4) yes . . . Pd1 C2 C1 72.4(3) yes . . . Pd1 C2 C3 104.9(4) yes . . . C1 C2 C3 107.6(5) yes . . . Pd1 C3 C2 102.6(4) yes 2_766 . . Pd1 C3 C4 75.0(4) yes 2_766 . . C2 C3 C4 107.0(4) yes . . . Pd1 C4 N1 106.4(3) yes 2_766 . . Pd1 C4 C3 69.3(3) yes 2_766 . . N1 C4 C3 108.1(5) yes . . . N2 C6 C7 178.2(7) yes . . . Pd1 C1 H1 91.479 no . . . N1 C1 H1 126.169 no . . . C2 C1 H1 126.173 no . . . Pd1 C2 H2 92.166 no . . . C1 C2 H2 126.223 no . . . C3 C2 H2 126.224 no . . . Pd1 C3 H3 92.016 no 2_766 . . C2 C3 H3 126.490 no . . . C4 C3 H3 126.494 no . . . Pd1 C4 H4 93.448 no 2_766 . . N1 C4 H4 125.954 no . . . C3 C4 H4 125.964 no . . . N1 C5 H5A 109.471 no . . . N1 C5 H5B 109.469 no . . . N1 C5 H5C 109.464 no . . . H5A C5 H5B 109.483 no . . . H5A C5 H5C 109.471 no . . . H5B C5 H5C 109.469 no . . . C6 C7 H7A 109.475 no . . . C6 C7 H7B 109.471 no . . . C6 C7 H7C 109.472 no . . . H7A C7 H7B 109.469 no . . . H7A C7 H7C 109.470 no . . . H7B C7 H7C 109.469 no . . . N3 C8 H8A 109.470 no . . . N3 C8 H8B 109.473 no . . . N3 C8 H8C 109.472 no . . . H8A C8 H8B 109.473 no . . . H8A C8 H8C 109.470 no . . . H8B C8 H8C 109.469 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Pd1 Pd1 C1 N1 35.6(3) no 2_766 . . . Pd1 Pd1 C1 C2 -68.03(18) no 2_766 . . . C1 Pd1 Pd1 C1 180(272009) no . . 2_766 2_766 C1 Pd1 Pd1 C2 -145.78(15) no . . 2_766 2_766 C1 Pd1 Pd1 C3 32.75(15) no . . 2_766 . C1 Pd1 Pd1 C4 -2.13(15) no . . 2_766 . Pd1 Pd1 C2 C1 106.4(3) no 2_766 . . . Pd1 Pd1 C2 C3 2.4(2) no 2_766 . . . C2 Pd1 Pd1 C1 145.78(13) no . . 2_766 2_766 C2 Pd1 Pd1 C2 -180(276639) no . . 2_766 2_766 C2 Pd1 Pd1 C3 -1.47(13) no . . 2_766 . C2 Pd1 Pd1 C4 -36.35(13) no . . 2_766 . Pd1 Pd1 C3 C2 -2.3(2) no 2_766 . 2_766 2_766 Pd1 Pd1 C3 C4 102.16(15) no 2_766 . 2_766 2_766 C3 Pd1 Pd1 C1 -32.75(13) no 2_766 . 2_766 2_766 C3 Pd1 Pd1 C2 1.47(13) no 2_766 . 2_766 2_766 C3 Pd1 Pd1 C3 -180(287167) no 2_766 . 2_766 . C3 Pd1 Pd1 C4 145.12(13) no 2_766 . 2_766 . Pd1 Pd1 C4 N1 30.6(3) no 2_766 . 2_766 2_766 Pd1 Pd1 C4 C3 -72.91(15) no 2_766 . 2_766 2_766 C4 Pd1 Pd1 C1 2.13(15) no 2_766 . 2_766 2_766 C4 Pd1 Pd1 C2 36.35(15) no 2_766 . 2_766 2_766 C4 Pd1 Pd1 C3 -145.12(15) no 2_766 . 2_766 . C4 Pd1 Pd1 C4 -180(188614) no 2_766 . 2_766 . N2 Pd1 C1 N1 -144.4(3) no . . . . N2 Pd1 C1 C2 112.0(3) no . . . . N2 Pd1 C2 C1 -73.4(3) no . . . . N2 Pd1 C2 C3 -177.4(3) no . . . . N2 Pd1 C3 C2 177.5(3) no . . 2_766 2_766 N2 Pd1 C3 C4 -78.02(19) no . . 2_766 2_766 N2 Pd1 C4 N1 -149.3(4) no . . 2_766 2_766 N2 Pd1 C4 C3 107.1(2) no . . 2_766 2_766 C1 Pd1 C2 C1 0.0(3) no . . . . C1 Pd1 C2 C3 -104.1(5) no . . . . C2 Pd1 C1 N1 103.6(4) no . . . . C2 Pd1 C1 C2 0.0(3) no . . . . C1 Pd1 C3 C2 64.5(4) no . . 2_766 2_766 C1 Pd1 C3 C4 168.99(18) no . . 2_766 2_766 C3 Pd1 C1 N1 -28.4(4) no 2_766 . . . C3 Pd1 C1 C2 -132.0(3) no 2_766 . . . C2 Pd1 C3 C2 -5.4(6) no . . 2_766 2_766 C2 Pd1 C3 C4 99.1(4) no . . 2_766 2_766 C3 Pd1 C2 C1 109.5(4) no 2_766 . . . C3 Pd1 C2 C3 5.5(6) no 2_766 . . . C2 Pd1 C4 N1 -31.5(6) no . . 2_766 2_766 C2 Pd1 C4 C3 -135.0(3) no . . 2_766 2_766 C4 Pd1 C2 C1 172.5(3) no 2_766 . . . C4 Pd1 C2 C3 68.4(5) no 2_766 . . . C3 Pd1 C4 N1 103.6(5) no 2_766 . 2_766 2_766 C3 Pd1 C4 C3 0.00(19) no 2_766 . 2_766 2_766 C4 Pd1 C3 C2 -104.5(4) no 2_766 . 2_766 2_766 C4 Pd1 C3 C4 -0.00(18) no 2_766 . 2_766 2_766 C1 N1 C4 Pd1 69.7(5) no . . . 2_766 C1 N1 C4 C3 -3.4(6) no . . . . C4 N1 C1 Pd1 -72.6(5) no . . . . C4 N1 C1 C2 3.0(6) no . . . . C5 N1 C1 Pd1 99.5(5) no . . . . C5 N1 C1 C2 175.1(5) no . . . . C5 N1 C4 Pd1 -102.5(5) no . . . 2_766 C5 N1 C4 C3 -175.6(4) no . . . . Pd1 C1 C2 Pd1 -0.0 no . . . . Pd1 C1 C2 C3 100.5(4) no . . . . N1 C1 C2 Pd1 -102.0(4) no . . . . N1 C1 C2 C3 -1.4(6) no . . . . Pd1 C2 C3 Pd1 -2.6(3) no . . . 2_766 Pd1 C2 C3 C4 75.3(4) no . . . . C1 C2 C3 Pd1 -78.5(4) no . . . 2_766 C1 C2 C3 C4 -0.6(6) no . . . . Pd1 C3 C4 Pd1 -0.0 no 2_766 . . 2_766 Pd1 C3 C4 N1 101.2(4) no 2_766 . . . C2 C3 C4 Pd1 -98.8(4) no . . . 2_766 C2 C3 C4 N1 2.4(6) 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 F1 O3 3.096(6) no . 2_755 F1 C3 3.233(7) no . 2_766 F1 C5 3.341(6) no . 1_655 F1 C7 3.388(7) no . 2_755 F1 C8 3.160(7) no . . F2 F4 3.240(4) no . 1_554 F2 C2 3.255(7) no . 1_554 F2 C5 3.369(7) no . 2_665 F2 C7 3.391(7) no . 2_755 F2 C8 3.257(8) no . . F3 C5 3.346(8) no . 2_765 F3 C7 3.269(6) no . 2_755 F3 C8 3.600(7) no . 2_765 F4 F2 3.240(4) no . 1_556 F4 O1 3.409(7) no . 1_556 F4 C4 3.361(7) no . 2_666 F4 C7 3.444(8) no . 2_656 F4 C8 3.515(7) no . 1_556 F5 O1 3.338(6) no . 2_655 F5 N2 3.126(7) no . . F5 C1 3.384(8) no . . F5 C2 3.284(7) no . . F5 C6 3.079(7) no . . F5 C6 3.503(6) no . 2_756 F5 C7 3.546(7) no . . F5 C7 3.427(6) no . 2_756 F6 O1 3.023(6) no . 2_655 F6 O3 3.202(7) no . 2_655 F6 N2 3.321(6) no . 1_455 F6 N3 2.861(6) no . 2_655 F6 C4 3.292(6) no . 2_666 F6 C6 3.289(6) no . 1_455 F6 C8 3.236(7) no . 2_655 O1 F4 3.409(7) no . 1_554 O1 F5 3.338(6) no . 2_655 O1 F6 3.023(6) no . 2_655 O1 O1 2.877(6) no . 2_655 O1 O3 3.445(7) no . 2_655 O1 N2 3.259(5) no . 2_655 O1 N3 3.011(7) no . 2_655 O1 C1 3.373(5) no . 2_655 O1 C6 3.070(6) no . 2_655 O1 C7 3.411(7) no . 2_655 O1 C8 3.506(9) no . 2_655 O3 F1 3.096(6) no . 2_755 O3 F6 3.202(7) no . 2_655 O3 O1 3.445(7) no . 2_655 N1 C2 3.499(7) no . 2_666 N1 C3 3.357(7) no . 2_666 N2 F5 3.126(7) no . . N2 F6 3.321(6) no . 1_655 N2 O1 3.259(5) no . 2_655 N3 F6 2.861(6) no . 2_655 N3 O1 3.011(7) no . 2_655 N3 N3 3.595(7) no . 2_655 C1 F5 3.384(8) no . . C1 O1 3.373(5) no . 2_655 C1 C3 3.571(7) no . 2_666 C1 C4 3.431(8) no . 2_666 C2 F2 3.255(7) no . 1_556 C2 F5 3.284(7) no . . C2 N1 3.499(7) no . 2_666 C2 C4 3.501(7) no . 2_666 C3 F1 3.233(7) no . 2_766 C3 N1 3.357(7) no . 2_666 C3 C1 3.571(7) no . 2_666 C4 F4 3.361(7) no . 2_666 C4 F6 3.292(6) no . 2_666 C4 C1 3.431(8) no . 2_666 C4 C2 3.501(7) no . 2_666 C5 F1 3.341(6) no . 1_455 C5 F2 3.369(7) no . 2_665 C5 F3 3.346(8) no . 2_765 C6 F5 3.079(7) no . . C6 F5 3.503(6) no . 2_756 C6 F6 3.289(6) no . 1_655 C6 O1 3.070(6) no . 2_655 C7 F1 3.388(7) no . 2_755 C7 F2 3.391(7) no . 2_755 C7 F3 3.269(6) no . 2_755 C7 F4 3.444(8) no . 2_656 C7 F5 3.546(7) no . . C7 F5 3.427(6) no . 2_756 C7 O1 3.411(7) no . 2_655 C8 F1 3.160(7) no . . C8 F2 3.257(8) no . . C8 F3 3.600(7) no . 2_765 C8 F4 3.515(7) no . 1_554 C8 F6 3.236(7) no . 2_655 C8 O1 3.506(9) no . 2_655 Pd1 H2 3.4774 no . 2_766 Pd1 H3 3.5762 no . . O1 H8A 2.5344 no . . O1 H8B 3.1138 no . . O1 H8C 2.6433 no . . O3 H8A 3.0103 no . . O3 H8B 2.4231 no . . O3 H8C 2.9082 no . . N1 H2 3.1564 no . . N1 H3 3.1590 no . . N2 H1 2.6938 no . . N2 H2 3.3007 no . . N2 H3 3.1823 no . 2_766 N2 H4 2.8043 no . 2_766 N2 H7A 3.0495 no . . N2 H7B 3.0308 no . . N2 H7C 3.0384 no . . C1 H3 3.1834 no . . C1 H4 3.1512 no . . C1 H5A 2.9340 no . . C1 H5B 3.2724 no . . C1 H5C 2.6739 no . . C2 H4 3.1752 no . . C3 H1 3.1822 no . . C4 H1 3.1515 no . . C4 H2 3.1764 no . . C4 H5A 2.9365 no . . C4 H5B 2.6444 no . . C4 H5C 3.2546 no . . C5 H1 2.8189 no . . C5 H4 2.7941 no . . C6 H1 3.3218 no . . C6 H4 3.5511 no . 2_766 H1 H2 2.5248 no . . H1 H5A 3.1505 no . . H1 H5C 2.6649 no . . H2 H3 2.5299 no . . H3 H4 2.5267 no . . H4 H5A 3.1519 no . . H4 H5B 2.6155 no . . P1 H2 3.5601 no . 1_554 P1 H2 3.5601 no . 2_766 P1 H5B 3.5570 no . 1_655 P1 H5B 3.5570 no . 2_665 P1 H7A 3.5032 no . 1_565 P1 H7A 3.5032 no . 2_755 P1 H8A 3.5136 no . . P1 H8A 3.5136 no . 2_765 P2 H4 3.3521 no . 1_545 P2 H4 3.3521 no . 2_666 F1 H2 3.3510 no . 2_766 F1 H3 2.4912 no . 2_766 F1 H5B 3.1089 no . 1_655 F1 H5C 2.6925 no . 1_655 F1 H7A 2.5994 no . 2_755 F1 H7C 3.3362 no . 2_755 F1 H8A 3.0423 no . . F1 H8B 2.6666 no . . F1 H8C 3.2692 no . . F2 H2 2.4899 no . 1_554 F2 H3 3.5424 no . 1_554 F2 H5B 2.5506 no . 2_665 F2 H5C 3.3639 no . 2_665 F2 H7A 3.1871 no . 2_755 F2 H7C 2.7138 no . 2_755 F2 H8A 2.4950 no . . F2 H8B 3.2885 no . . F2 H8C 3.5760 no . . F3 H2 3.0981 no . 1_554 F3 H3 3.4190 no . 1_554 F3 H5A 2.3759 no . 2_765 F3 H5B 3.2502 no . 1_655 F3 H5C 3.3976 no . 1_655 F3 H7A 2.9233 no . 2_755 F3 H7B 3.3467 no . 2_755 F3 H7C 3.0030 no . 2_755 F3 H8A 3.2346 no . 2_765 F3 H8C 3.2870 no . 2_765 F4 H2 3.4887 no . . F4 H4 2.5326 no . 2_666 F4 H5B 2.8255 no . 2_666 F4 H7B 2.5171 no . 2_656 F4 H8A 2.6592 no . 1_556 F5 H1 2.9319 no . . F5 H2 2.7144 no . . F5 H7B 3.0138 no . . F5 H7C 2.6169 no . 2_756 F6 H1 3.3114 no . . F6 H4 2.4600 no . 2_666 F6 H7C 3.3273 no . 1_455 F6 H8A 2.8388 no . 2_655 F6 H8B 3.4658 no . 2_655 O1 H1 2.4364 no . 2_655 O1 H7A 3.2765 no . 2_655 O1 H7B 3.2742 no . 2_655 O1 H8C 2.9898 no . 2_655 O3 H1 3.1078 no . 2_655 O3 H3 2.8986 no . 1_544 O3 H5C 2.7963 no . 2_655 O3 H7A 2.7875 no . . O3 H8B 2.7463 no . 2_755 N1 H3 3.5623 no . 2_666 N2 H7B 3.4846 no . 2_756 N2 H7C 3.3729 no . 2_756 N2 H8C 3.3308 no . . N3 H1 3.0961 no . 2_655 N3 H5C 3.5869 no . 2_655 N3 H7A 3.5488 no . . C1 H4 3.5423 no . 2_666 C2 H5B 3.4684 no . 2_666 C3 H5C 3.4520 no . 2_666 C5 H3 3.5939 no . 2_666 C5 H8C 3.4312 no . . H1 F5 2.9319 no . . H1 F6 3.3114 no . . H1 O1 2.4364 no . 2_655 H1 O3 3.1078 no . 2_655 H1 N3 3.0961 no . 2_655 H1 H8C 3.1584 no . . H2 P1 3.5601 no . 1_556 H2 F1 3.3510 no . 2_766 H2 F2 2.4899 no . 1_556 H2 F3 3.0981 no . 1_556 H2 F4 3.4887 no . . H2 F5 2.7144 no . . H2 H5B 3.2507 no . 2_666 H2 H7C 2.7179 no . 2_756 H3 F1 2.4912 no . 2_766 H3 F2 3.5424 no . 1_556 H3 F3 3.4190 no . 1_556 H3 O3 2.8986 no . 1_566 H3 N1 3.5623 no . 2_666 H3 C5 3.5939 no . 2_666 H3 H5B 3.5995 no . 2_666 H3 H5C 3.1099 no . 2_666 H3 H8B 3.1905 no . 2_766 H3 H8C 3.3265 no . 2_766 H4 P2 3.3521 no . 1_565 H4 F4 2.5326 no . 2_666 H4 F6 2.4600 no . 2_666 H4 C1 3.5423 no . 2_666 H4 H7B 3.1426 no . 1_565 H5A F3 2.3759 no . 2_765 H5A H7B 3.4401 no . 1_565 H5A H8A 3.5939 no . . H5A H8C 2.9200 no . . H5B P1 3.5570 no . 1_455 H5B F1 3.1089 no . 1_455 H5B F2 2.5506 no . 2_665 H5B F3 3.2502 no . 1_455 H5B F4 2.8255 no . 2_666 H5B C2 3.4684 no . 2_666 H5B H2 3.2507 no . 2_666 H5B H3 3.5995 no . 2_666 H5B H7B 3.3641 no . 1_565 H5B H8A 3.5007 no . 2_665 H5C F1 2.6925 no . 1_455 H5C F2 3.3639 no . 2_665 H5C F3 3.3976 no . 1_455 H5C O3 2.7963 no . 2_655 H5C N3 3.5869 no . 2_655 H5C C3 3.4520 no . 2_666 H5C H3 3.1099 no . 2_666 H5C H7A 3.1791 no . 2_655 H5C H8C 3.1934 no . . H7A P1 3.5032 no . 1_545 H7A F1 2.5994 no . 2_755 H7A F2 3.1871 no . 2_755 H7A F3 2.9233 no . 2_755 H7A O1 3.2765 no . 2_655 H7A O3 2.7875 no . . H7A N3 3.5488 no . . H7A H5C 3.1791 no . 2_655 H7A H8B 3.0908 no . 2_755 H7B F3 3.3467 no . 2_755 H7B F4 2.5171 no . 2_656 H7B F5 3.0138 no . . H7B O1 3.2742 no . 2_655 H7B N2 3.4846 no . 2_756 H7B H4 3.1426 no . 1_545 H7B H5A 3.4401 no . 1_545 H7B H5B 3.3641 no . 1_545 H7C F1 3.3362 no . 2_755 H7C F2 2.7138 no . 2_755 H7C F3 3.0030 no . 2_755 H7C F5 2.6169 no . 2_756 H7C F6 3.3273 no . 1_655 H7C N2 3.3729 no . 2_756 H7C H2 2.7179 no . 2_756 H7C H8A 3.5065 no . 2_755 H8A P1 3.5136 no . . H8A F1 3.0423 no . . H8A F2 2.4950 no . . H8A F3 3.2346 no . 2_765 H8A F4 2.6592 no . 1_554 H8A F6 2.8388 no . 2_655 H8A H5A 3.5939 no . . H8A H5B 3.5007 no . 2_665 H8A H7C 3.5065 no . 2_755 H8B F1 2.6666 no . . H8B F2 3.2885 no . . H8B F6 3.4658 no . 2_655 H8B O3 2.7463 no . 2_755 H8B H3 3.1905 no . 2_766 H8B H7A 3.0908 no . 2_755 H8B H8B 3.1053 no . 2_755 H8C F1 3.2692 no . . H8C F2 3.5760 no . . H8C F3 3.2870 no . 2_765 H8C O1 2.9898 no . 2_655 H8C N2 3.3308 no . . H8C C5 3.4312 no . . H8C H1 3.1584 no . . H8C H3 3.3265 no . 2_766 H8C H5A 2.9200 no . . H8C H5C 3.1934 no . . data_indole_Pd2_CH3CN_PF6 _database_code_depnum_ccdc_archive 'CCDC 904115' #TrackingRef 'CCDC 904115 4-Ci.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C20 H20 F12 N4 P2 Pd2' _chemical_formula_moiety 'C20 H20 F12 N4 P2 Pd2' _chemical_formula_weight 819.13 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.934(2) _cell_length_b 8.982(3) _cell_length_c 9.950(3) _cell_angle_alpha 103.254(2) _cell_angle_beta 107.386(3) _cell_angle_gamma 101.872(2) _cell_volume 629.3(3) _cell_formula_units_Z 1 _cell_measurement_reflns_used 1865 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 27.49 _cell_measurement_temperature 123 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.040 _exptl_crystal_density_diffrn 2.161 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 398.00 _exptl_absorpt_coefficient_mu 1.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.936 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 123 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.629 _diffrn_reflns_number 3875 _diffrn_reflns_av_R_equivalents 0.0122 _diffrn_reflns_theta_max 24.18 _diffrn_reflns_theta_full 24.18 _diffrn_measured_fraction_theta_max 0.961 _diffrn_measured_fraction_theta_full 0.961 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1938 _reflns_number_gt 1837 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0815 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 1938 _refine_ls_number_parameters 181 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0393P)^2^+2.0658P] where P=(Fo^2^+2Fc^2^)/3' _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 0.990 _refine_diff_density_min -0.570 _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) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.1023 0.0942 ; 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 0.17330(4) 0.04085(4) 0.07757(4) 0.02687(15) Uani 1.0 2 d . . . P1 P 0.36190(17) 0.26988(15) 0.57841(14) 0.0348(3) Uani 1.0 2 d . . . F1 F 0.1660(4) 0.2092(5) 0.5916(4) 0.0535(9) Uani 1.0 2 d . . . F2 F 0.5585(5) 0.3237(6) 0.5652(5) 0.0732(12) Uani 1.0 2 d . . . F3 F 0.2659(6) 0.2750(6) 0.4183(4) 0.0752(12) Uani 1.0 2 d . . . F4 F 0.4563(6) 0.2567(9) 0.7371(5) 0.114(2) Uani 1.0 2 d . . . F5 F 0.3753(8) 0.4467(5) 0.6472(7) 0.117(2) Uani 1.0 2 d . . . F6 F 0.3518(7) 0.0901(5) 0.5064(6) 0.0896(14) Uani 1.0 2 d . . . N1 N 0.4606(6) 0.1078(5) 0.1961(5) 0.0323(9) Uani 1.0 2 d . . . N2 N 0.0917(8) 0.4601(6) 0.2226(6) 0.0506(13) Uani 1.0 2 d . . . C1 C -0.0752(10) 0.4806(7) 0.2036(7) 0.0525(15) Uani 1.0 2 d . . . C2 C -0.2037(9) 0.3827(7) 0.0688(8) 0.0526(17) Uani 1.0 2 d . . . C3 C -0.1073(7) 0.2945(6) -0.0034(6) 0.0348(12) Uani 1.0 2 d . . . C4 C -0.1529(7) 0.1811(6) -0.1434(6) 0.0340(12) Uani 1.0 2 d . . . C5 C -0.0132(7) 0.1265(6) -0.1790(5) 0.0331(11) Uani 1.0 2 d . . . C6 C 0.1718(7) 0.1855(6) -0.0771(6) 0.0312(11) Uani 1.0 2 d . . . C7 C 0.2164(7) 0.2940(6) 0.0635(6) 0.0321(11) Uani 1.0 2 d . . . C8 C 0.0756(7) 0.3472(5) 0.0978(5) 0.0319(11) Uani 1.0 2 d . . . C9 C 0.6070(8) 0.1482(6) 0.2713(6) 0.0356(12) Uani 1.0 2 d . . . C10 C 0.7982(7) 0.1992(8) 0.3714(7) 0.0520(15) Uani 1.0 2 d . . . H1 H -0.1015 0.5537 0.2744 0.0631 Uiso 1.0 2 calc R . . H2 H 0.1931 0.5101 0.3011 0.0607 Uiso 1.0 2 calc R . . H2A H -0.3312 0.3751 0.0310 0.0632 Uiso 1.0 2 calc R . . H4 H -0.2766 0.1425 -0.2125 0.0408 Uiso 1.0 2 calc R . . H5 H -0.0430 0.0493 -0.2722 0.0397 Uiso 1.0 2 calc R . . H6 H 0.2661 0.1514 -0.1041 0.0374 Uiso 1.0 2 calc R . . H7 H 0.3392 0.3305 0.1338 0.0385 Uiso 1.0 2 calc R . . H10A H 0.8140 0.1321 0.4366 0.0624 Uiso 1.0 2 calc R . . H10B H 0.8314 0.3113 0.4314 0.0624 Uiso 1.0 2 calc R . . H10C H 0.8785 0.1887 0.3139 0.0624 Uiso 1.0 2 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 0.0207(3) 0.0242(2) 0.0303(3) 0.00193(14) 0.00188(15) 0.01249(15) P1 0.0238(7) 0.0397(8) 0.0331(7) 0.0040(6) 0.0019(6) 0.0125(6) F1 0.0282(17) 0.074(3) 0.0527(19) 0.0086(15) 0.0116(15) 0.0204(17) F2 0.037(2) 0.099(3) 0.067(3) -0.0019(19) 0.0196(18) 0.013(3) F3 0.065(3) 0.118(4) 0.050(2) 0.031(3) 0.0126(19) 0.046(3) F4 0.053(3) 0.254(7) 0.052(3) 0.052(4) 0.015(2) 0.077(4) F5 0.127(5) 0.049(3) 0.163(5) 0.010(3) 0.081(4) -0.012(3) F6 0.112(4) 0.055(3) 0.136(4) 0.041(3) 0.074(4) 0.040(3) N1 0.029(3) 0.029(2) 0.041(3) 0.0059(18) 0.012(2) 0.0175(18) N2 0.072(4) 0.035(3) 0.043(3) 0.015(3) 0.019(3) 0.012(2) C1 0.071(5) 0.043(4) 0.056(4) 0.020(3) 0.032(4) 0.022(3) C2 0.044(4) 0.052(4) 0.098(5) 0.028(3) 0.041(4) 0.057(4) C3 0.033(3) 0.028(3) 0.052(3) 0.012(2) 0.016(3) 0.025(3) C4 0.022(3) 0.030(3) 0.045(3) 0.0008(19) -0.002(2) 0.025(3) C5 0.044(3) 0.023(3) 0.028(3) 0.002(2) 0.010(3) 0.0117(19) C6 0.031(3) 0.030(3) 0.038(3) 0.009(2) 0.013(3) 0.020(2) C7 0.028(3) 0.026(3) 0.038(3) 0.0022(19) 0.002(2) 0.020(2) C8 0.042(3) 0.021(3) 0.029(3) 0.005(2) 0.008(3) 0.0118(19) C9 0.035(4) 0.033(3) 0.043(3) 0.010(3) 0.013(3) 0.021(3) C10 0.022(3) 0.060(4) 0.061(4) 0.000(3) -0.003(3) 0.030(3) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'DIRDIF99-PATTY (Gould, et al., 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _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 Pd1 2.5683(8) yes . 2_555 Pd1 N1 2.110(5) yes . . Pd1 C4 2.227(6) yes . 2_555 Pd1 C5 2.360(6) yes . 2_555 Pd1 C6 2.229(6) yes . . Pd1 C7 2.272(5) yes . . P1 F1 1.592(4) yes . . P1 F2 1.589(5) yes . . P1 F3 1.563(5) yes . . P1 F4 1.576(6) yes . . P1 F5 1.546(5) yes . . P1 F6 1.584(5) yes . . N1 C9 1.106(7) yes . . N2 C1 1.338(10) yes . . N2 C8 1.365(7) yes . . C1 C2 1.373(8) yes . . C2 C3 1.430(10) yes . . C3 C4 1.416(7) yes . . C3 C8 1.403(7) yes . . C4 C5 1.405(9) yes . . C5 C6 1.417(7) yes . . C6 C7 1.403(7) yes . . C7 C8 1.402(9) yes . . C9 C10 1.451(7) yes . . N2 H2 0.880 no . . C1 H1 0.950 no . . C2 H2A 0.950 no . . C4 H4 0.950 no . . C5 H5 0.950 no . . C6 H6 0.950 no . . C7 H7 0.950 no . . C10 H10A 0.980 no . . C10 H10B 0.980 no . . C10 H10C 0.980 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 Pd1 Pd1 N1 177.37(14) yes 2_555 . . Pd1 Pd1 C4 93.89(12) yes 2_555 . 2_555 Pd1 Pd1 C5 71.96(12) yes 2_555 . 2_555 Pd1 Pd1 C6 78.73(12) yes 2_555 . . Pd1 Pd1 C7 92.27(12) yes 2_555 . . N1 Pd1 C4 87.31(17) yes . . 2_555 N1 Pd1 C5 110.20(18) yes . . 2_555 N1 Pd1 C6 99.25(18) yes . . . N1 Pd1 C7 86.99(17) yes . . . C4 Pd1 C5 35.5(2) yes 2_555 . 2_555 C4 Pd1 C6 155.83(18) yes 2_555 . . C4 Pd1 C7 167.71(18) yes 2_555 . . C5 Pd1 C6 150.25(18) yes 2_555 . . C5 Pd1 C7 138.7(2) yes 2_555 . . C6 Pd1 C7 36.31(17) yes . . . F1 P1 F2 177.7(3) yes . . . F1 P1 F3 90.7(3) yes . . . F1 P1 F4 88.7(3) yes . . . F1 P1 F5 91.6(3) yes . . . F1 P1 F6 89.7(3) yes . . . F2 P1 F3 90.1(3) yes . . . F2 P1 F4 90.4(3) yes . . . F2 P1 F5 90.4(3) yes . . . F2 P1 F6 88.3(3) yes . . . F3 P1 F4 177.5(4) yes . . . F3 P1 F5 91.7(3) yes . . . F3 P1 F6 87.9(3) yes . . . F4 P1 F5 90.7(4) yes . . . F4 P1 F6 89.8(4) yes . . . F5 P1 F6 178.6(4) yes . . . Pd1 N1 C9 172.5(6) yes . . . C1 N2 C8 107.4(5) yes . . . N2 C1 C2 111.4(7) yes . . . C1 C2 C3 106.3(6) yes . . . C2 C3 C4 135.8(5) yes . . . C2 C3 C8 104.9(5) yes . . . C4 C3 C8 119.3(6) yes . . . Pd1 C4 C3 99.3(4) yes 2_555 . . Pd1 C4 C5 77.4(4) yes 2_555 . . C3 C4 C5 119.2(4) yes . . . Pd1 C5 C4 67.1(4) yes 2_555 . . Pd1 C5 C6 105.2(4) yes 2_555 . . C4 C5 C6 120.5(5) yes . . . Pd1 C6 C5 103.1(4) yes . . . Pd1 C6 C7 73.5(4) yes . . . C5 C6 C7 120.4(6) yes . . . Pd1 C7 C6 70.2(3) yes . . . Pd1 C7 C8 106.4(4) yes . . . C6 C7 C8 118.5(4) yes . . . N2 C8 C3 110.0(6) yes . . . N2 C8 C7 127.8(5) yes . . . C3 C8 C7 122.1(5) yes . . . N1 C9 C10 179.0(7) yes . . . C1 N2 H2 126.318 no . . . C8 N2 H2 126.320 no . . . N2 C1 H1 124.297 no . . . C2 C1 H1 124.294 no . . . C1 C2 H2A 126.831 no . . . C3 C2 H2A 126.828 no . . . Pd1 C4 H4 93.171 no 2_555 . . C3 C4 H4 120.396 no . . . C5 C4 H4 120.394 no . . . Pd1 C5 H5 97.390 no 2_555 . . C4 C5 H5 119.736 no . . . C6 C5 H5 119.733 no . . . Pd1 C6 H6 93.263 no . . . C5 C6 H6 119.814 no . . . C7 C6 H6 119.814 no . . . Pd1 C7 H7 93.134 no . . . C6 C7 H7 120.760 no . . . C8 C7 H7 120.764 no . . . C9 C10 H10A 109.471 no . . . C9 C10 H10B 109.471 no . . . C9 C10 H10C 109.474 no . . . H10A C10 H10B 109.471 no . . . H10A C10 H10C 109.471 no . . . H10B C10 H10C 109.469 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Pd1 Pd1 C4 C3 67.0(3) no 2_555 . 2_555 2_555 Pd1 Pd1 C4 C5 -50.99(16) no 2_555 . 2_555 2_555 C4 Pd1 Pd1 C4 180(278599) no 2_555 . 2_555 . C4 Pd1 Pd1 C5 -151.65(15) no 2_555 . 2_555 . C4 Pd1 Pd1 C6 23.23(15) no 2_555 . 2_555 2_555 C4 Pd1 Pd1 C7 -10.64(15) no 2_555 . 2_555 2_555 Pd1 Pd1 C5 C4 125.38(16) no 2_555 . 2_555 2_555 Pd1 Pd1 C5 C6 8.2(3) no 2_555 . 2_555 2_555 C5 Pd1 Pd1 C4 151.65(13) no 2_555 . 2_555 . C5 Pd1 Pd1 C5 180(265962) no 2_555 . 2_555 . C5 Pd1 Pd1 C6 -5.12(13) no 2_555 . 2_555 2_555 C5 Pd1 Pd1 C7 -38.99(13) no 2_555 . 2_555 2_555 Pd1 Pd1 C6 C5 -8.3(3) no 2_555 . . . Pd1 Pd1 C6 C7 109.8(2) no 2_555 . . . C6 Pd1 Pd1 C4 -23.23(14) no . . 2_555 . C6 Pd1 Pd1 C5 5.12(14) no . . 2_555 . C6 Pd1 Pd1 C6 180(271030) no . . 2_555 2_555 C6 Pd1 Pd1 C7 146.12(14) no . . 2_555 2_555 Pd1 Pd1 C7 C6 -67.39(19) no 2_555 . . . Pd1 Pd1 C7 C8 47.6(3) no 2_555 . . . C7 Pd1 Pd1 C4 10.64(15) no . . 2_555 . C7 Pd1 Pd1 C5 38.99(15) no . . 2_555 . C7 Pd1 Pd1 C6 -146.12(15) no . . 2_555 2_555 C7 Pd1 Pd1 C7 180(268460) no . . 2_555 2_555 N1 Pd1 C4 C3 -110.6(3) no . . 2_555 2_555 N1 Pd1 C4 C5 131.3(2) no . . 2_555 2_555 N1 Pd1 C5 C4 -53.0(2) no . . 2_555 2_555 N1 Pd1 C5 C6 -170.2(3) no . . 2_555 2_555 N1 Pd1 C6 C5 170.0(3) no . . . . N1 Pd1 C6 C7 -71.9(3) no . . . . N1 Pd1 C7 C6 110.1(3) no . . . . N1 Pd1 C7 C8 -134.9(3) no . . . . C4 Pd1 C5 C4 0.00(18) no 2_555 . 2_555 2_555 C4 Pd1 C5 C6 -117.2(4) no 2_555 . 2_555 2_555 C5 Pd1 C4 C3 118.0(4) no 2_555 . 2_555 2_555 C5 Pd1 C4 C5 0.00(17) no 2_555 . 2_555 2_555 C4 Pd1 C6 C5 65.7(6) no 2_555 . . . C4 Pd1 C6 C7 -176.1(4) no 2_555 . . . C6 Pd1 C4 C3 -3.9(6) no . . 2_555 2_555 C6 Pd1 C4 C5 -121.9(5) no . . 2_555 2_555 C5 Pd1 C6 C5 -18.2(6) no 2_555 . . . C5 Pd1 C6 C7 100.0(3) no 2_555 . . . C6 Pd1 C5 C4 135.5(3) no . . 2_555 2_555 C6 Pd1 C5 C6 18.3(6) no . . 2_555 2_555 C5 Pd1 C7 C6 -132.3(3) no 2_555 . . . C5 Pd1 C7 C8 -17.3(4) no 2_555 . . . C7 Pd1 C5 C4 -162.50(17) no . . 2_555 2_555 C7 Pd1 C5 C6 80.3(3) no . . 2_555 2_555 C6 Pd1 C7 C6 0.0(3) no . . . . C6 Pd1 C7 C8 115.0(4) no . . . . C7 Pd1 C6 C5 -118.2(5) no . . . . C7 Pd1 C6 C7 0.0(3) no . . . . C1 N2 C8 C3 -0.1(7) no . . . . C1 N2 C8 C7 175.7(6) no . . . . C8 N2 C1 C2 0.5(8) no . . . . N2 C1 C2 C3 -0.7(8) no . . . . C1 C2 C3 C4 -176.8(6) no . . . . C1 C2 C3 C8 0.6(7) no . . . . C2 C3 C4 Pd1 -103.4(8) no . . . 2_555 C2 C3 C4 C5 175.9(7) no . . . . C2 C3 C8 N2 -0.4(7) no . . . . C2 C3 C8 C7 -176.4(5) no . . . . C4 C3 C8 N2 177.6(5) no . . . . C4 C3 C8 C7 1.5(8) no . . . . C8 C3 C4 Pd1 79.4(6) no . . . 2_555 C8 C3 C4 C5 -1.3(8) no . . . . Pd1 C4 C5 Pd1 0.0 no 2_555 . . 2_555 Pd1 C4 C5 C6 -94.6(5) no 2_555 . . . C3 C4 C5 Pd1 93.8(5) no . . . 2_555 C3 C4 C5 C6 -0.8(8) no . . . . Pd1 C5 C6 Pd1 9.2(4) no 2_555 . . . Pd1 C5 C6 C7 -69.2(5) no 2_555 . . . C4 C5 C6 Pd1 81.3(6) no . . . . C4 C5 C6 C7 2.9(8) no . . . . Pd1 C6 C7 Pd1 0.0 no . . . . Pd1 C6 C7 C8 -98.4(4) no . . . . C5 C6 C7 Pd1 95.8(5) no . . . . C5 C6 C7 C8 -2.6(8) no . . . . Pd1 C7 C8 N2 109.1(5) no . . . . Pd1 C7 C8 C3 -75.6(5) no . . . . C6 C7 C8 N2 -174.9(5) no . . . . C6 C7 C8 C3 0.4(8) 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 Pd1 C3 3.557(6) no . . Pd1 C8 3.378(4) no . 2_555 N2 C4 3.592(6) no . . C1 C7 3.544(10) no . . C2 C7 3.595(10) no . . C3 C6 2.816(9) no . . C4 C7 2.841(6) no . . C5 C8 2.788(7) no . . Pd1 F3 3.326(4) no . . F1 C1 3.396(8) no . 2_566 F1 C5 3.173(8) no . 1_556 F1 C6 3.340(7) no . 1_556 F1 C10 3.050(7) no . 1_455 F2 F3 3.534(7) no . 2_666 F2 F5 3.348(9) no . 2_666 F2 N1 3.502(6) no . . F2 N2 2.887(6) no . 2_666 F2 C9 3.161(8) no . . F2 C10 3.265(9) no . . F3 Pd1 3.326(4) no . . F3 F2 3.534(7) no . 2_666 F3 N1 3.317(7) no . . F3 N2 3.048(8) no . . F3 C5 3.595(6) no . 2_555 F3 C7 3.482(7) no . . F3 C8 3.368(7) no . . F3 C10 3.497(8) no . 1_455 F4 C2 3.340(7) no . 1_656 F4 C3 3.541(7) no . 1_656 F4 C4 3.243(8) no . 1_656 F4 C6 3.371(8) no . 1_556 F4 C9 3.545(10) no . 2_656 F5 F2 3.348(9) no . 2_666 F5 C1 3.257(11) no . 2_566 F5 C7 3.529(6) no . 2_666 F5 C9 3.505(8) no . 2_666 F6 F6 3.133(8) no . 2_656 F6 N1 3.474(9) no . . F6 C4 3.528(7) no . 2_555 F6 C5 3.366(6) no . 2_555 F6 C9 3.577(10) no . . F6 C9 3.407(9) no . 2_656 F6 C10 3.269(9) no . 2_656 N1 F2 3.502(6) no . . N1 F3 3.317(7) no . . N1 F6 3.474(9) no . . N2 F2 2.887(6) no . 2_666 N2 F3 3.048(8) no . . N2 C3 3.448(9) no . 2_565 N2 C4 3.463(8) no . 2_565 C1 F1 3.396(8) no . 2_566 C1 F5 3.257(11) no . 2_566 C1 C3 3.537(10) no . 2_565 C1 C4 3.476(9) no . 2_565 C1 C5 3.533(9) no . 2_565 C1 C10 3.476(11) no . 1_455 C2 F4 3.340(7) no . 1_454 C2 C7 3.459(10) no . 2_565 C2 C8 3.391(10) no . 2_565 C3 F4 3.541(7) no . 1_454 C3 N2 3.448(9) no . 2_565 C3 C1 3.537(10) no . 2_565 C3 C8 3.535(8) no . 2_565 C4 F4 3.243(8) no . 1_454 C4 F6 3.528(7) no . 2_555 C4 N2 3.463(8) no . 2_565 C4 C1 3.476(9) no . 2_565 C5 F1 3.173(8) no . 1_554 C5 F3 3.595(6) no . 2_555 C5 F6 3.366(6) no . 2_555 C5 C1 3.533(9) no . 2_565 C6 F1 3.340(7) no . 1_554 C6 F4 3.371(8) no . 1_554 C7 F3 3.482(7) no . . C7 F5 3.529(6) no . 2_666 C7 C2 3.459(10) no . 2_565 C8 F3 3.368(7) no . . C8 C2 3.391(10) no . 2_565 C8 C3 3.535(8) no . 2_565 C9 F2 3.161(8) no . . C9 F4 3.545(10) no . 2_656 C9 F5 3.505(8) no . 2_666 C9 F6 3.577(10) no . . C9 F6 3.407(9) no . 2_656 C10 F1 3.050(7) no . 1_655 C10 F2 3.265(9) no . . C10 F3 3.497(8) no . 1_655 C10 F6 3.269(9) no . 2_656 C10 C1 3.476(11) no . 1_655 Pd1 H5 3.4161 no . . N1 H4 2.4844 no . 2_555 N1 H6 3.0799 no . . N1 H7 2.5140 no . . N1 H10A 3.0217 no . . N1 H10B 3.0306 no . . N1 H10C 3.0313 no . . N2 H2A 3.1513 no . . N2 H7 2.7384 no . . C2 H2 3.0850 no . . C2 H4 2.9283 no . . C3 H1 3.1609 no . . C3 H2 3.1153 no . . C3 H5 3.2925 no . . C3 H7 3.3095 no . . C4 H2A 3.0238 no . . C4 H6 3.3034 no . . C5 H7 3.3076 no . . C6 H4 3.3090 no . . C7 H2 2.7748 no . . C7 H5 3.2993 no . . C8 H1 3.0914 no . . C8 H2A 3.1702 no . . C8 H4 3.2934 no . . C8 H6 3.2708 no . . C9 H4 3.0981 no . 2_555 C9 H7 3.1284 no . . H1 H2 2.3957 no . . H1 H2A 2.4775 no . . H2 H7 2.7222 no . . H2A H4 3.0170 no . . H4 H5 2.3570 no . . H5 H6 2.3607 no . . H6 H7 2.3613 no . . P1 H1 3.3188 no . 2_566 P1 H2 3.3647 no . 2_666 P1 H4 3.5693 no . 1_656 P1 H5 3.5084 no . 2_555 P1 H10A 3.5445 no . 2_656 F1 H1 2.4755 no . 2_566 F1 H5 2.8113 no . 1_556 F1 H5 3.2054 no . 2_555 F1 H6 3.0865 no . 1_556 F1 H10A 2.6075 no . 1_455 F1 H10A 3.0558 no . 2_656 F1 H10B 3.0937 no . 1_455 F1 H10C 2.9492 no . 1_455 F2 H2 2.0478 no . 2_666 F2 H4 3.1701 no . 1_656 F2 H7 3.5384 no . 2_666 F2 H10A 3.2680 no . . F2 H10B 2.8674 no . . F3 H2 2.7171 no . . F3 H5 2.8513 no . 2_555 F3 H7 3.1802 no . . F3 H10B 3.5668 no . 1_455 F3 H10C 2.8053 no . 1_455 F4 H1 3.5647 no . 2_566 F4 H2 3.2970 no . 2_666 F4 H2A 2.7223 no . 1_656 F4 H4 2.5076 no . 1_656 F4 H6 2.6817 no . 1_556 F4 H7 3.4820 no . 2_666 F4 H10A 3.4231 no . 2_656 F5 H1 2.5180 no . 2_566 F5 H2 3.5401 no . . F5 H2 3.2324 no . 2_666 F5 H2A 3.3899 no . 2_566 F5 H7 2.6585 no . 2_666 F5 H10B 3.0828 no . 2_666 F6 H4 3.2610 no . 1_656 F6 H4 2.9861 no . 2_555 F6 H5 2.6440 no . 2_555 F6 H10A 2.4337 no . 2_656 N2 H10B 3.3805 no . 2_666 N2 H10C 3.1407 no . 1_455 C1 H10B 3.1819 no . 1_455 C1 H10B 3.4100 no . 2_666 C1 H10C 3.0628 no . 1_455 C2 H10C 3.2981 no . 1_455 C3 H10C 3.5253 no . 1_455 C4 H1 3.5300 no . 2_565 C4 H2 3.5089 no . 2_565 C5 H1 3.2663 no . 2_565 C5 H10C 3.3635 no . 2_655 C6 H1 3.4123 no . 2_565 C6 H10C 3.5014 no . 2_655 C7 H2A 3.3503 no . 2_565 C8 H2A 3.5932 no . 2_565 C8 H10C 3.4049 no . 1_455 C9 H2A 3.5550 no . 1_655 C9 H6 3.3299 no . 2_655 C10 H1 3.5397 no . 1_655 C10 H1 3.5050 no . 2_666 C10 H5 3.4127 no . 2_655 C10 H6 3.4555 no . 2_655 H1 P1 3.3188 no . 2_566 H1 F1 2.4755 no . 2_566 H1 F4 3.5647 no . 2_566 H1 F5 2.5180 no . 2_566 H1 C4 3.5300 no . 2_565 H1 C5 3.2663 no . 2_565 H1 C6 3.4123 no . 2_565 H1 C10 3.5397 no . 1_455 H1 C10 3.5050 no . 2_666 H1 H5 3.5205 no . 2_565 H1 H10A 3.3388 no . 2_666 H1 H10B 3.0078 no . 1_455 H1 H10B 2.8614 no . 2_666 H1 H10C 3.3681 no . 1_455 H2 P1 3.3647 no . 2_666 H2 F2 2.0478 no . 2_666 H2 F3 2.7171 no . . H2 F4 3.2970 no . 2_666 H2 F5 3.5401 no . . H2 F5 3.2324 no . 2_666 H2 C4 3.5089 no . 2_565 H2 H4 3.4221 no . 2_565 H2 H10B 2.8587 no . 2_666 H2 H10C 3.4602 no . 1_455 H2A F4 2.7223 no . 1_454 H2A F5 3.3899 no . 2_566 H2A C7 3.3503 no . 2_565 H2A C8 3.5932 no . 2_565 H2A C9 3.5550 no . 1_455 H2A H6 3.0990 no . 1_455 H2A H7 3.0657 no . 1_455 H2A H7 3.4169 no . 2_565 H4 P1 3.5693 no . 1_454 H4 F2 3.1701 no . 1_454 H4 F4 2.5076 no . 1_454 H4 F6 3.2610 no . 1_454 H4 F6 2.9861 no . 2_555 H4 H2 3.4221 no . 2_565 H5 P1 3.5084 no . 2_555 H5 F1 2.8113 no . 1_554 H5 F1 3.2054 no . 2_555 H5 F3 2.8513 no . 2_555 H5 F6 2.6440 no . 2_555 H5 C10 3.4127 no . 2_655 H5 H1 3.5205 no . 2_565 H5 H10A 3.0996 no . 1_454 H5 H10A 3.2254 no . 2_655 H5 H10C 2.7401 no . 2_655 H6 F1 3.0865 no . 1_554 H6 F4 2.6817 no . 1_554 H6 C9 3.3299 no . 2_655 H6 C10 3.4555 no . 2_655 H6 H2A 3.0990 no . 1_655 H6 H10A 3.4714 no . 2_655 H6 H10C 3.0343 no . 2_655 H7 F2 3.5384 no . 2_666 H7 F3 3.1802 no . . H7 F4 3.4820 no . 2_666 H7 F5 2.6585 no . 2_666 H7 H2A 3.0657 no . 1_655 H7 H2A 3.4169 no . 2_565 H10A P1 3.5445 no . 2_656 H10A F1 2.6075 no . 1_655 H10A F1 3.0558 no . 2_656 H10A F2 3.2680 no . . H10A F4 3.4231 no . 2_656 H10A F6 2.4337 no . 2_656 H10A H1 3.3388 no . 2_666 H10A H5 3.0996 no . 1_656 H10A H5 3.2254 no . 2_655 H10A H6 3.4714 no . 2_655 H10B F1 3.0937 no . 1_655 H10B F2 2.8674 no . . H10B F3 3.5668 no . 1_655 H10B F5 3.0828 no . 2_666 H10B N2 3.3805 no . 2_666 H10B C1 3.1819 no . 1_655 H10B C1 3.4100 no . 2_666 H10B H1 3.0078 no . 1_655 H10B H1 2.8614 no . 2_666 H10B H2 2.8587 no . 2_666 H10B H10B 3.5326 no . 2_766 H10C F1 2.9492 no . 1_655 H10C F3 2.8053 no . 1_655 H10C N2 3.1407 no . 1_655 H10C C1 3.0628 no . 1_655 H10C C2 3.2981 no . 1_655 H10C C3 3.5253 no . 1_655 H10C C5 3.3635 no . 2_655 H10C C6 3.5014 no . 2_655 H10C C8 3.4049 no . 1_655 H10C H1 3.3681 no . 1_655 H10C H2 3.4602 no . 1_655 H10C H5 2.7401 no . 2_655 H10C H6 3.0343 no . 2_655 #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag N2 H2 F2 . . 2_666 2.887(6) 0.880 2.048 159.0 no #============================================================================== # 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 #==============================================================================