# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Raithby, Paul' 'Warren, Mark' 'Brayshaw, Simon' 'Hatcher, Lauren' 'Johnson, Andrew' 'Schiffers, Stefanie' 'Woodall, Christopher' 'Teat, Simon' 'Warren, John' 'Warren, Anna' _publ_contact_author_name 'Raithby, Paul' _publ_contact_author_email p.r.raithby@bath.ac.uk _publ_section_title ; Photoactivated Linkage Isomerism in Single Crystals of Nickel, Palladium and Platinum Di-nitro Complexes - A Photocrystallographic Investigation ; _publ_requested_category FM # Attachment '- all_1_4_cif.cif.txt' data_1_GS _database_code_depnum_ccdc_archive 'CCDC 866979' #TrackingRef '- all_1_4_cif.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis-(Triethylphosphine)dinitro-nickel(II) ; _chemical_formula_moiety 'C12 H30 N2 Ni O4 P2' _chemical_formula_sum 'C12 H30 N2 Ni O4 P2' _chemical_formula_weight 387.03 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.839(4) _cell_length_b 7.814(4) _cell_length_c 15.152(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.15(4) _cell_angle_gamma 90.00 _cell_volume 924.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9601 _cell_measurement_theta_min 3.60 _cell_measurement_theta_max 29.77 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_special_details ; ? ; _exptl_absorpt_coefficient_mu 1.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9408 _exptl_absorpt_correction_T_max 0.9638 _exptl_absorpt_process_details ; SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.69450 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'beamline 9.8, DLS' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9601 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 29.77 _reflns_number_total 2731 _reflns_number_gt 2332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+0.7284P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2731 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.206 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ni1 Ni 0.5000 0.0000 0.0000 0.01311(11) Uani 1 2 d S . . P1 P 0.70737(7) -0.15152(7) 0.07430(3) 0.01396(13) Uani 1 1 d . . . O1 O 0.2971(2) -0.2784(2) -0.01775(12) 0.0275(4) Uani 1 1 d . . . N1 N 0.3343(2) -0.1556(2) 0.03154(12) 0.0164(4) Uani 1 1 d . . . C1 C 0.6383(3) -0.3436(3) 0.12994(15) 0.0201(4) Uani 1 1 d . . . H1A H 0.5485 -0.3107 0.1687 0.024 Uiso 1 1 calc R . . H1B H 0.5853 -0.4229 0.0844 0.024 Uiso 1 1 calc R . . O2 O 0.2675(2) -0.1352(2) 0.10127(11) 0.0271(4) Uani 1 1 d . . . C2 C 0.7790(3) -0.4396(3) 0.18581(17) 0.0269(5) Uani 1 1 d . . . H2A H 0.8683 -0.4746 0.1482 0.040 Uiso 1 1 calc R . . H2B H 0.7302 -0.5413 0.2119 0.040 Uiso 1 1 calc R . . H2C H 0.8288 -0.3647 0.2332 0.040 Uiso 1 1 calc R . . C3 C 0.8223(3) -0.0214(3) 0.16028(14) 0.0199(4) Uani 1 1 d . . . H3A H 0.9089 -0.0930 0.1945 0.024 Uiso 1 1 calc R . . H3B H 0.8831 0.0722 0.1322 0.024 Uiso 1 1 calc R . . C4 C 0.7003(3) 0.0553(3) 0.22338(15) 0.0261(5) Uani 1 1 d . . . H4A H 0.6161 0.1284 0.1898 0.039 Uiso 1 1 calc R . . H4B H 0.7660 0.1236 0.2688 0.039 Uiso 1 1 calc R . . H4C H 0.6409 -0.0372 0.2518 0.039 Uiso 1 1 calc R . . C5 C 0.8684(3) -0.2215(3) 0.00312(15) 0.0192(4) Uani 1 1 d . . . H5A H 0.9262 -0.1198 -0.0193 0.023 Uiso 1 1 calc R . . H5B H 0.9558 -0.2903 0.0385 0.023 Uiso 1 1 calc R . . C6 C 0.7937(3) -0.3276(3) -0.07525(16) 0.0251(5) Uani 1 1 d . . . H6A H 0.7519 -0.4369 -0.0539 0.038 Uiso 1 1 calc R . . H6B H 0.8826 -0.3492 -0.1154 0.038 Uiso 1 1 calc R . . H6C H 0.6986 -0.2651 -0.1069 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01128(19) 0.0138(2) 0.01434(18) 0.00126(14) 0.00182(13) -0.00108(14) P1 0.0125(3) 0.0146(3) 0.0149(2) 0.00011(19) 0.00137(19) -0.0002(2) O1 0.0265(9) 0.0193(9) 0.0359(10) 0.0002(7) -0.0020(7) -0.0048(7) N1 0.0128(8) 0.0173(9) 0.0185(9) 0.0042(7) -0.0021(7) 0.0022(7) C1 0.0194(11) 0.0181(11) 0.0226(11) 0.0052(8) 0.0005(8) -0.0011(8) O2 0.0215(9) 0.0348(10) 0.0259(9) 0.0093(7) 0.0066(7) 0.0004(7) C2 0.0282(13) 0.0232(12) 0.0285(12) 0.0090(10) -0.0025(10) 0.0052(10) C3 0.0202(11) 0.0209(11) 0.0178(10) -0.0027(8) -0.0025(8) -0.0001(9) C4 0.0362(14) 0.0259(12) 0.0163(11) -0.0041(9) 0.0032(9) 0.0044(11) C5 0.0152(10) 0.0204(11) 0.0225(11) -0.0010(9) 0.0049(8) 0.0007(8) C6 0.0293(13) 0.0223(12) 0.0243(11) -0.0047(9) 0.0057(10) 0.0004(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.8725(19) 3_655 ? Ni1 N1 1.8725(19) . ? Ni1 P1 2.2325(10) 3_655 ? Ni1 P1 2.2325(10) . ? P1 C5 1.817(2) . ? P1 C3 1.825(2) . ? P1 C1 1.828(2) . ? O1 N1 1.234(2) . ? N1 O2 1.231(2) . ? C1 C2 1.526(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.533(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.522(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 180.00(15) 3_655 . ? N1 Ni1 P1 90.99(6) 3_655 3_655 ? N1 Ni1 P1 89.01(6) . 3_655 ? N1 Ni1 P1 89.01(6) 3_655 . ? N1 Ni1 P1 90.99(6) . . ? P1 Ni1 P1 180.00(3) 3_655 . ? C5 P1 C3 105.47(11) . . ? C5 P1 C1 106.08(11) . . ? C3 P1 C1 106.03(11) . . ? C5 P1 Ni1 111.94(9) . . ? C3 P1 Ni1 110.79(9) . . ? C1 P1 Ni1 115.83(8) . . ? O2 N1 O1 121.63(19) . . ? O2 N1 Ni1 119.54(16) . . ? O1 N1 Ni1 118.82(15) . . ? C2 C1 P1 115.48(17) . . ? C2 C1 H1A 108.4 . . ? P1 C1 H1A 108.4 . . ? C2 C1 H1B 108.4 . . ? P1 C1 H1B 108.4 . . ? H1A C1 H1B 107.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 111.55(17) . . ? C4 C3 H3A 109.3 . . ? P1 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? P1 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P1 112.85(16) . . ? C6 C5 H5A 109.0 . . ? P1 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? P1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 P1 C5 -58.52(10) 3_655 . . . ? N1 Ni1 P1 C5 121.48(10) . . . . ? P1 Ni1 P1 C5 34(100) 3_655 . . . ? N1 Ni1 P1 C3 58.91(11) 3_655 . . . ? N1 Ni1 P1 C3 -121.09(11) . . . . ? P1 Ni1 P1 C3 151(100) 3_655 . . . ? N1 Ni1 P1 C1 179.70(10) 3_655 . . . ? N1 Ni1 P1 C1 -0.30(10) . . . . ? P1 Ni1 P1 C1 -88(100) 3_655 . . . ? N1 Ni1 N1 O2 172(100) 3_655 . . . ? P1 Ni1 N1 O2 -91.69(16) 3_655 . . . ? P1 Ni1 N1 O2 88.31(16) . . . . ? N1 Ni1 N1 O1 -7(100) 3_655 . . . ? P1 Ni1 N1 O1 89.58(16) 3_655 . . . ? P1 Ni1 N1 O1 -90.42(16) . . . . ? C5 P1 C1 C2 59.2(2) . . . . ? C3 P1 C1 C2 -52.6(2) . . . . ? Ni1 P1 C1 C2 -175.93(15) . . . . ? C5 P1 C3 C4 177.03(16) . . . . ? C1 P1 C3 C4 -70.72(19) . . . . ? Ni1 P1 C3 C4 55.72(18) . . . . ? C3 P1 C5 C6 -177.90(17) . . . . ? C1 P1 C5 C6 69.90(19) . . . . ? Ni1 P1 C5 C6 -57.33(18) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 29.77 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.592 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.109 ###END data_1_es _database_code_depnum_ccdc_archive 'CCDC 866980' #TrackingRef '- all_1_4_cif.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis-(Triethylphosphine)dinitro-nickel(II) ; _chemical_formula_moiety 'C12 H30 N2 Ni O4 P2' _chemical_formula_sum 'C12 H30 N2 Ni O4 P2' _chemical_formula_weight 387.03 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.890(4) _cell_length_b 7.787(3) _cell_length_c 15.251(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.82(2) _cell_angle_gamma 90.00 _cell_volume 933.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9782 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 29.77 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_special_details ; ? ; _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9413 _exptl_absorpt_correction_T_max 0.9642 _exptl_absorpt_process_details ; SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.69450 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline 9.8, DLS' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9782 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 29.77 _reflns_number_total 2743 _reflns_number_gt 2449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.3051P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2743 _refine_ls_number_parameters 125 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ni1 Ni 0.5000 0.0000 0.0000 0.02046(9) Uani 1 2 d SD . . P1 P 0.70616(5) -0.15087(5) 0.07317(3) 0.02189(10) Uani 1 1 d . A . C1 C 0.6402(2) -0.3447(2) 0.12875(13) 0.0320(4) Uani 1 1 d . . . H1A H 0.5521 -0.3126 0.1683 0.038 Uiso 1 1 calc R A . H1B H 0.5870 -0.4242 0.0838 0.038 Uiso 1 1 calc R . . C2 C 0.7814(3) -0.4401(3) 0.18234(16) 0.0437(5) Uani 1 1 d . A . H2A H 0.8664 -0.4790 0.1434 0.066 Uiso 1 1 calc R . . H2B H 0.7335 -0.5397 0.2108 0.066 Uiso 1 1 calc R . . H2C H 0.8352 -0.3633 0.2273 0.066 Uiso 1 1 calc R . . C3 C 0.8193(2) -0.0193(2) 0.15783(11) 0.0292(3) Uani 1 1 d . . . H3A H 0.9076 -0.0899 0.1908 0.035 Uiso 1 1 calc R A . H3B H 0.8772 0.0761 0.1295 0.035 Uiso 1 1 calc R . . C4 C 0.6999(3) 0.0542(3) 0.22192(12) 0.0391(4) Uani 1 1 d . A . H4A H 0.6151 0.1279 0.1899 0.059 Uiso 1 1 calc R . . H4B H 0.7656 0.1219 0.2670 0.059 Uiso 1 1 calc R . . H4C H 0.6422 -0.0399 0.2500 0.059 Uiso 1 1 calc R . . C5 C 0.8658(2) -0.2193(2) 0.00168(12) 0.0295(3) Uani 1 1 d . . . H5A H 0.9218 -0.1166 -0.0210 0.035 Uiso 1 1 calc R A . H5B H 0.9537 -0.2872 0.0365 0.035 Uiso 1 1 calc R . . C6 C 0.7927(3) -0.3271(3) -0.07591(14) 0.0402(4) Uani 1 1 d . A . H6A H 0.7525 -0.4372 -0.0544 0.060 Uiso 1 1 calc R . . H6B H 0.8812 -0.3478 -0.1161 0.060 Uiso 1 1 calc R . . H6C H 0.6975 -0.2657 -0.1072 0.060 Uiso 1 1 calc R . . N1 N 0.3341(4) -0.1566(4) 0.0313(2) 0.0219(6) Uani 0.748(3) 1 d PD A 1 O2 O 0.2695(3) -0.1363(4) 0.10203(18) 0.0312(5) Uani 0.748(3) 1 d PD A 1 O1 O 0.2977(2) -0.2794(2) -0.01658(13) 0.0353(5) Uani 0.748(3) 1 d PD A 1 O2A O 0.3125(18) -0.0867(19) 0.1301(8) 0.057(3) Uiso 0.160(5) 1 d PD A 2 N1A N 0.267(2) -0.202(2) 0.0759(9) 0.054(4) Uiso 0.160(5) 1 d PD A 2 O1A O 0.3321(19) -0.2009(17) 0.0063(8) 0.057(3) Uiso 0.160(5) 1 d PD A 2 O2B O 0.182(2) -0.208(2) 0.1323(11) 0.051(6) Uiso 0.091(5) 1 d PD A 3 N1B N 0.292(4) -0.094(3) 0.104(2) 0.035(6) Uiso 0.091(5) 1 d PD A 3 O1B O 0.345(4) -0.132(4) 0.042(2) 0.035(6) Uiso 0.091(5) 1 d PD A 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01972(15) 0.01777(14) 0.02441(15) 0.00336(10) 0.00486(10) -0.00063(9) P1 0.02092(19) 0.01963(19) 0.0255(2) 0.00230(14) 0.00437(14) 0.00073(14) C1 0.0298(8) 0.0258(8) 0.0406(9) 0.0125(7) 0.0048(7) 0.0010(6) C2 0.0422(11) 0.0341(10) 0.0539(12) 0.0173(9) -0.0011(9) 0.0069(9) C3 0.0320(9) 0.0283(8) 0.0271(8) -0.0018(6) 0.0008(6) 0.0011(6) C4 0.0524(12) 0.0387(10) 0.0270(9) -0.0017(7) 0.0077(8) 0.0088(9) C5 0.0250(8) 0.0288(8) 0.0358(9) -0.0030(7) 0.0085(6) 0.0024(6) C6 0.0444(11) 0.0343(10) 0.0432(11) -0.0117(8) 0.0117(9) 0.0013(8) N1 0.0182(10) 0.0178(14) 0.0291(15) 0.0053(10) -0.0010(10) -0.0005(8) O2 0.0268(11) 0.0333(15) 0.0347(12) 0.0109(11) 0.0104(9) -0.0041(10) O1 0.0380(10) 0.0198(9) 0.0469(11) 0.0007(7) -0.0032(8) -0.0073(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1B 1.755(10) 3_655 ? Ni1 O1B 1.755(10) . ? Ni1 N1 1.879(2) 3_655 ? Ni1 N1 1.879(2) . ? Ni1 O1A 2.058(10) 3_655 ? Ni1 O1A 2.058(10) . ? Ni1 P1 2.2285(8) 3_655 ? Ni1 P1 2.2285(8) . ? P1 C5 1.8140(18) . ? P1 C3 1.8220(18) . ? P1 C1 1.8278(18) . ? C1 C2 1.519(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.525(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.524(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? N1 O1 1.222(4) . ? N1 O2 1.242(3) . ? O2A N1A 1.253(10) . ? N1A O1A 1.218(10) . ? O2B N1B 1.333(11) . ? N1B O1B 1.114(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1B Ni1 O1B 180.0(14) 3_655 . ? O1B Ni1 N1 7.4(10) 3_655 3_655 ? O1B Ni1 N1 172.6(10) . 3_655 ? O1B Ni1 N1 172.6(10) 3_655 . ? O1B Ni1 N1 7.4(10) . . ? N1 Ni1 N1 180.00(17) 3_655 . ? O1B Ni1 O1A 21.4(10) 3_655 3_655 ? O1B Ni1 O1A 158.6(10) . 3_655 ? N1 Ni1 O1A 14.1(3) 3_655 3_655 ? N1 Ni1 O1A 165.9(3) . 3_655 ? O1B Ni1 O1A 158.6(10) 3_655 . ? O1B Ni1 O1A 21.4(10) . . ? N1 Ni1 O1A 165.9(3) 3_655 . ? N1 Ni1 O1A 14.1(3) . . ? O1A Ni1 O1A 180.0(5) 3_655 . ? O1B Ni1 P1 90.5(14) 3_655 3_655 ? O1B Ni1 P1 89.5(14) . 3_655 ? N1 Ni1 P1 91.45(12) 3_655 3_655 ? N1 Ni1 P1 88.55(12) . 3_655 ? O1A Ni1 P1 91.2(5) 3_655 3_655 ? O1A Ni1 P1 88.8(5) . 3_655 ? O1B Ni1 P1 89.5(14) 3_655 . ? O1B Ni1 P1 90.5(14) . . ? N1 Ni1 P1 88.55(12) 3_655 . ? N1 Ni1 P1 91.45(12) . . ? O1A Ni1 P1 88.8(5) 3_655 . ? O1A Ni1 P1 91.2(5) . . ? P1 Ni1 P1 180.00(2) 3_655 . ? C5 P1 C3 105.51(9) . . ? C5 P1 C1 105.97(9) . . ? C3 P1 C1 106.09(9) . . ? C5 P1 Ni1 111.62(7) . . ? C3 P1 Ni1 110.62(7) . . ? C1 P1 Ni1 116.32(6) . . ? C2 C1 P1 115.42(14) . . ? C2 C1 H1A 108.4 . . ? P1 C1 H1A 108.4 . . ? C2 C1 H1B 108.4 . . ? P1 C1 H1B 108.4 . . ? H1A C1 H1B 107.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 111.89(14) . . ? C4 C3 H3A 109.2 . . ? P1 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? P1 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P1 113.07(13) . . ? C6 C5 H5A 109.0 . . ? P1 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? P1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 N1 O2 121.7(2) . . ? O1 N1 Ni1 119.3(2) . . ? O2 N1 Ni1 118.9(2) . . ? O1A N1A O2A 116.7(12) . . ? N1A O1A Ni1 111.6(8) . . ? O1B N1B O2B 113.5(14) . . ? N1B O1B Ni1 118.9(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1B Ni1 P1 C5 -51.2(9) 3_655 . . . ? O1B Ni1 P1 C5 128.8(9) . . . . ? N1 Ni1 P1 C5 -58.47(13) 3_655 . . . ? N1 Ni1 P1 C5 121.53(13) . . . . ? O1A Ni1 P1 C5 -72.5(3) 3_655 . . . ? O1A Ni1 P1 C5 107.5(3) . . . . ? P1 Ni1 P1 C5 130(100) 3_655 . . . ? O1B Ni1 P1 C3 66.0(9) 3_655 . . . ? O1B Ni1 P1 C3 -114.0(9) . . . . ? N1 Ni1 P1 C3 58.69(13) 3_655 . . . ? N1 Ni1 P1 C3 -121.31(13) . . . . ? O1A Ni1 P1 C3 44.6(3) 3_655 . . . ? O1A Ni1 P1 C3 -135.4(3) . . . . ? P1 Ni1 P1 C3 -113(100) 3_655 . . . ? O1B Ni1 P1 C1 -172.9(9) 3_655 . . . ? O1B Ni1 P1 C1 7.1(9) . . . . ? N1 Ni1 P1 C1 179.79(13) 3_655 . . . ? N1 Ni1 P1 C1 -0.21(13) . . . . ? O1A Ni1 P1 C1 165.7(3) 3_655 . . . ? O1A Ni1 P1 C1 -14.3(3) . . . . ? P1 Ni1 P1 C1 8(100) 3_655 . . . ? C5 P1 C1 C2 58.55(18) . . . . ? C3 P1 C1 C2 -53.28(17) . . . . ? Ni1 P1 C1 C2 -176.76(13) . . . . ? C5 P1 C3 C4 177.88(13) . . . . ? C1 P1 C3 C4 -69.96(15) . . . . ? Ni1 P1 C3 C4 57.02(14) . . . . ? C3 P1 C5 C6 -178.02(14) . . . . ? C1 P1 C5 C6 69.73(15) . . . . ? Ni1 P1 C5 C6 -57.81(15) . . . . ? O1B Ni1 N1 O1 7(12) 3_655 . . . ? O1B Ni1 N1 O1 -173(12) . . . . ? N1 Ni1 N1 O1 -174(65) 3_655 . . . ? O1A Ni1 N1 O1 179(2) 3_655 . . . ? O1A Ni1 N1 O1 -1(2) . . . . ? P1 Ni1 N1 O1 90.0(3) 3_655 . . . ? P1 Ni1 N1 O1 -90.0(3) . . . . ? O1B Ni1 N1 O2 -176(12) 3_655 . . . ? O1B Ni1 N1 O2 4(12) . . . . ? N1 Ni1 N1 O2 3(65) 3_655 . . . ? O1A Ni1 N1 O2 -4(2) 3_655 . . . ? O1A Ni1 N1 O2 176(2) . . . . ? P1 Ni1 N1 O2 -92.9(3) 3_655 . . . ? P1 Ni1 N1 O2 87.1(3) . . . . ? O2A N1A O1A Ni1 -1(2) . . . . ? O1B Ni1 O1A N1A 175(4) 3_655 . . . ? O1B Ni1 O1A N1A -5(4) . . . . ? N1 Ni1 O1A N1A 172.5(13) 3_655 . . . ? N1 Ni1 O1A N1A -7.5(13) . . . . ? O1A Ni1 O1A N1A 17(100) 3_655 . . . ? P1 Ni1 O1A N1A -96.4(14) 3_655 . . . ? P1 Ni1 O1A N1A 83.6(14) . . . . ? O2B N1B O1B Ni1 -177(3) . . . . ? O1B Ni1 O1B N1B 15(100) 3_655 . . . ? N1 Ni1 O1B N1B 8(16) 3_655 . . . ? N1 Ni1 O1B N1B -172(16) . . . . ? O1A Ni1 O1B N1B 3(8) 3_655 . . . ? O1A Ni1 O1B N1B -177(8) . . . . ? P1 Ni1 O1B N1B -89(4) 3_655 . . . ? P1 Ni1 O1B N1B 91(4) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 29.77 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.427 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.056 ###END data_2_gs _database_code_depnum_ccdc_archive 'CCDC 866981' #TrackingRef '- all_1_4_cif.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis-(Triphenylphosphine)dinitro-palladium(II) ; _chemical_formula_moiety 'C38 H34 Cl4 N2 O4 P2 Pd' _chemical_formula_sum 'C38 H34 Cl4 N2 O4 P2 Pd' _chemical_formula_weight 892.81 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.690(18) _cell_length_b 8.069(7) _cell_length_c 23.51(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3925(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8483 _cell_measurement_theta_min 3.49 _cell_measurement_theta_max 33.19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9720 _exptl_absorpt_correction_T_max 0.9905 _exptl_absorpt_process_details ; SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline 13.3.1, ALS' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33795 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 33.36 _reflns_number_total 5807 _reflns_number_gt 4748 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1134P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5807 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1184 0.1127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.7856 1.1793 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.0000 0.5000 0.0000 0.01558(11) Uani 1 2 d S . . Cl21 Cl -0.14608(4) 0.12752(10) 0.27375(3) 0.04289(19) Uani 1 1 d . . . Cl22 Cl -0.26549(4) 0.25888(11) 0.32627(4) 0.0510(2) Uani 1 1 d . . . P1 P 0.06376(2) 0.65368(6) -0.06569(2) 0.01574(13) Uani 1 1 d . . . O1 O -0.05830(9) 0.3642(2) -0.09848(7) 0.0302(4) Uani 1 1 d . . . O2 O -0.12087(8) 0.5469(3) -0.05857(8) 0.0319(4) Uani 1 1 d . . . N1 N -0.06943(9) 0.4680(3) -0.06008(8) 0.0213(4) Uani 1 1 d . . . C1 C 0.02232(10) 0.7789(3) -0.12059(8) 0.0183(4) Uani 1 1 d . . . C2 C -0.01618(12) 0.7000(3) -0.16207(9) 0.0252(4) Uani 1 1 d . . . H2 H -0.0206 0.5828 -0.1615 0.030 Uiso 1 1 calc R . . C3 C -0.04794(12) 0.7923(3) -0.20414(10) 0.0303(5) Uani 1 1 d . . . H3 H -0.0740 0.7380 -0.2317 0.036 Uiso 1 1 calc R . . C4 C -0.04112(13) 0.9652(4) -0.20546(11) 0.0317(5) Uani 1 1 d . . . H4 H -0.0624 1.0280 -0.2340 0.038 Uiso 1 1 calc R . . C5 C -0.00287(12) 1.0452(4) -0.16472(12) 0.0305(6) Uani 1 1 d . . . H5 H 0.0018 1.1622 -0.1658 0.037 Uiso 1 1 calc R . . C6 C 0.02878(11) 0.9527(3) -0.12218(9) 0.0238(4) Uani 1 1 d . . . H6 H 0.0545 1.0076 -0.0945 0.029 Uiso 1 1 calc R . . C7 C 0.11458(10) 0.5111(2) -0.10682(10) 0.0183(4) Uani 1 1 d . . . C8 C 0.14329(11) 0.5621(3) -0.15848(9) 0.0234(4) Uani 1 1 d . . . H8 H 0.1370 0.6721 -0.1717 0.028 Uiso 1 1 calc R . . C9 C 0.18103(12) 0.4512(3) -0.19035(10) 0.0276(5) Uani 1 1 d . . . H9 H 0.1996 0.4855 -0.2254 0.033 Uiso 1 1 calc R . . C10 C 0.19124(12) 0.2889(3) -0.17023(11) 0.0277(5) Uani 1 1 d . . . H10 H 0.2168 0.2137 -0.1917 0.033 Uiso 1 1 calc R . . C11 C 0.16374(12) 0.2380(3) -0.11853(11) 0.0272(5) Uani 1 1 d . . . H11 H 0.1712 0.1289 -0.1049 0.033 Uiso 1 1 calc R . . C12 C 0.12505(11) 0.3483(3) -0.08677(10) 0.0226(4) Uani 1 1 d . . . H12 H 0.1061 0.3132 -0.0520 0.027 Uiso 1 1 calc R . . C13 C 0.11773(9) 0.7988(2) -0.02841(9) 0.0174(4) Uani 1 1 d . . . C14 C 0.18508(10) 0.8009(3) -0.03663(10) 0.0228(4) Uani 1 1 d . . . H14 H 0.2044 0.7278 -0.0633 0.027 Uiso 1 1 calc R . . C15 C 0.22387(13) 0.9117(3) -0.00515(10) 0.0291(5) Uani 1 1 d . . . H15 H 0.2694 0.9120 -0.0102 0.035 Uiso 1 1 calc R . . C16 C 0.19505(13) 1.0219(3) 0.03367(12) 0.0293(5) Uani 1 1 d . . . H16 H 0.2213 1.0975 0.0543 0.035 Uiso 1 1 calc R . . C17 C 0.12783(13) 1.0212(3) 0.04215(11) 0.0264(5) Uani 1 1 d . . . H17 H 0.1085 1.0967 0.0681 0.032 Uiso 1 1 calc R . . C18 C 0.08937(11) 0.9078(3) 0.01190(10) 0.0220(4) Uani 1 1 d . . . H18 H 0.0441 0.9041 0.0185 0.026 Uiso 1 1 calc R . . C21 C -0.18366(16) 0.2019(4) 0.33742(12) 0.0413(7) Uani 1 1 d . . . H21A H -0.1816 0.1145 0.3669 0.050 Uiso 1 1 calc R . . H21B H -0.1594 0.2992 0.3516 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01136(17) 0.01823(18) 0.01715(17) 0.00013(6) -0.00057(6) -0.00146(6) Cl21 0.0500(4) 0.0435(4) 0.0352(3) 0.0082(3) 0.0028(3) -0.0027(3) Cl22 0.0454(4) 0.0607(5) 0.0471(4) -0.0032(3) -0.0183(3) 0.0209(3) P1 0.0117(2) 0.0165(3) 0.0190(2) 0.00018(17) 0.00022(17) -0.00045(16) O1 0.0335(9) 0.0317(9) 0.0253(8) -0.0057(6) -0.0040(7) -0.0024(7) O2 0.0214(8) 0.0399(10) 0.0343(9) 0.0001(8) -0.0076(7) 0.0050(7) N1 0.0182(9) 0.0257(9) 0.0201(8) 0.0012(7) -0.0032(7) -0.0046(7) C1 0.0132(9) 0.0219(10) 0.0200(9) 0.0011(7) 0.0013(7) 0.0021(7) C2 0.0246(11) 0.0271(11) 0.0238(10) 0.0024(8) -0.0038(9) -0.0023(9) C3 0.0280(12) 0.0386(13) 0.0242(10) 0.0038(9) -0.0069(9) 0.0020(10) C4 0.0317(13) 0.0368(13) 0.0264(11) 0.0080(10) -0.0032(10) 0.0107(10) C5 0.0395(16) 0.0235(12) 0.0284(13) 0.0047(11) 0.0016(9) 0.0079(9) C6 0.0246(11) 0.0208(10) 0.0261(10) 0.0000(8) -0.0005(8) 0.0043(8) C7 0.0134(10) 0.0194(10) 0.0220(10) -0.0019(7) -0.0003(8) 0.0016(6) C8 0.0236(10) 0.0225(11) 0.0242(10) 0.0007(8) 0.0053(8) 0.0003(8) C9 0.0238(11) 0.0329(12) 0.0262(11) -0.0031(9) 0.0066(8) 0.0022(9) C10 0.0204(11) 0.0290(12) 0.0336(11) -0.0086(9) 0.0019(9) 0.0054(8) C11 0.0245(11) 0.0206(10) 0.0364(12) -0.0019(8) -0.0006(9) 0.0052(8) C12 0.0194(10) 0.0222(10) 0.0261(10) 0.0023(8) 0.0005(8) 0.0013(7) C13 0.0131(9) 0.0171(9) 0.0221(9) 0.0009(7) -0.0005(7) -0.0004(6) C14 0.0155(9) 0.0229(10) 0.0302(10) 0.0002(8) 0.0006(8) -0.0017(7) C15 0.0182(11) 0.0317(13) 0.0374(13) -0.0003(9) -0.0032(8) -0.0067(9) C16 0.0286(13) 0.0272(11) 0.0321(12) -0.0011(9) -0.0060(10) -0.0108(9) C17 0.0292(12) 0.0233(11) 0.0268(11) -0.0027(8) -0.0011(9) -0.0009(8) C18 0.0189(10) 0.0213(10) 0.0257(9) -0.0005(8) 0.0003(8) -0.0002(8) C21 0.0409(16) 0.0513(17) 0.0317(13) 0.0004(12) -0.0101(11) 0.0064(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.031(2) 5_565 ? Pd1 N1 2.031(2) . ? Pd1 P1 2.3798(13) 5_565 ? Pd1 P1 2.3798(13) . ? Cl21 C21 1.790(3) . ? Cl22 C21 1.774(3) . ? P1 C7 1.834(2) . ? P1 C13 1.840(2) . ? P1 C1 1.850(2) . ? O1 N1 1.253(3) . ? O2 N1 1.241(3) . ? C1 C6 1.409(3) . ? C1 C2 1.411(3) . ? C2 C3 1.402(3) . ? C2 H2 0.9500 . ? C3 C4 1.402(4) . ? C3 H3 0.9500 . ? C4 C5 1.400(4) . ? C4 H4 0.9500 . ? C5 C6 1.409(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.412(3) . ? C7 C8 1.413(3) . ? C8 C9 1.404(3) . ? C8 H8 0.9500 . ? C9 C10 1.408(4) . ? C9 H9 0.9500 . ? C10 C11 1.403(4) . ? C10 H10 0.9500 . ? C11 C12 1.411(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.407(3) . ? C13 C18 1.420(3) . ? C14 C15 1.411(3) . ? C14 H14 0.9500 . ? C15 C16 1.407(4) . ? C15 H15 0.9500 . ? C16 C17 1.405(4) . ? C16 H16 0.9500 . ? C17 C18 1.406(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.00(16) 5_565 . ? N1 Pd1 P1 90.40(8) 5_565 5_565 ? N1 Pd1 P1 89.60(8) . 5_565 ? N1 Pd1 P1 89.60(8) 5_565 . ? N1 Pd1 P1 90.40(8) . . ? P1 Pd1 P1 180.000(19) 5_565 . ? C7 P1 C13 107.60(11) . . ? C7 P1 C1 103.93(11) . . ? C13 P1 C1 105.41(11) . . ? C7 P1 Pd1 109.44(9) . . ? C13 P1 Pd1 111.03(9) . . ? C1 P1 Pd1 118.72(9) . . ? O2 N1 O1 121.41(19) . . ? O2 N1 Pd1 121.45(16) . . ? O1 N1 Pd1 117.13(15) . . ? C6 C1 C2 119.0(2) . . ? C6 C1 P1 121.22(16) . . ? C2 C1 P1 119.79(17) . . ? C3 C2 C1 120.8(2) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 119.8(2) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.0(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 120.1(2) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C12 C7 C8 119.6(2) . . ? C12 C7 P1 119.70(18) . . ? C8 C7 P1 120.74(16) . . ? C9 C8 C7 120.4(2) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.8(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 120.1(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 119.8(2) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C14 C13 C18 119.58(19) . . ? C14 C13 P1 122.89(16) . . ? C18 C13 P1 117.47(16) . . ? C13 C14 C15 119.9(2) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.0(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.6(2) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 119.4(2) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C17 C18 C13 120.5(2) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? Cl22 C21 Cl21 112.20(16) . . ? Cl22 C21 H21A 109.2 . . ? Cl21 C21 H21A 109.2 . . ? Cl22 C21 H21B 109.2 . . ? Cl21 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 P1 C7 92.62(10) 5_565 . . . ? N1 Pd1 P1 C7 -87.38(10) . . . . ? P1 Pd1 P1 C7 30(5) 5_565 . . . ? N1 Pd1 P1 C13 -26.02(9) 5_565 . . . ? N1 Pd1 P1 C13 153.98(9) . . . . ? P1 Pd1 P1 C13 -89(5) 5_565 . . . ? N1 Pd1 P1 C1 -148.39(10) 5_565 . . . ? N1 Pd1 P1 C1 31.61(10) . . . . ? P1 Pd1 P1 C1 149(6) 5_565 . . . ? N1 Pd1 N1 O2 -134(100) 5_565 . . . ? P1 Pd1 N1 O2 74.82(18) 5_565 . . . ? P1 Pd1 N1 O2 -105.18(18) . . . . ? N1 Pd1 N1 O1 46(100) 5_565 . . . ? P1 Pd1 N1 O1 -104.58(17) 5_565 . . . ? P1 Pd1 N1 O1 75.42(17) . . . . ? C7 P1 C1 C6 -121.29(19) . . . . ? C13 P1 C1 C6 -8.2(2) . . . . ? Pd1 P1 C1 C6 116.90(17) . . . . ? C7 P1 C1 C2 58.2(2) . . . . ? C13 P1 C1 C2 171.28(18) . . . . ? Pd1 P1 C1 C2 -63.58(19) . . . . ? C6 C1 C2 C3 -0.4(3) . . . . ? P1 C1 C2 C3 -179.88(19) . . . . ? C1 C2 C3 C4 0.5(4) . . . . ? C2 C3 C4 C5 -0.2(4) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C2 C1 C6 C5 0.0(3) . . . . ? P1 C1 C6 C5 179.48(17) . . . . ? C4 C5 C6 C1 0.3(4) . . . . ? C13 P1 C7 C12 103.27(19) . . . . ? C1 P1 C7 C12 -145.26(18) . . . . ? Pd1 P1 C7 C12 -17.5(2) . . . . ? C13 P1 C7 C8 -76.9(2) . . . . ? C1 P1 C7 C8 34.6(2) . . . . ? Pd1 P1 C7 C8 162.35(16) . . . . ? C12 C7 C8 C9 1.2(3) . . . . ? P1 C7 C8 C9 -178.66(18) . . . . ? C7 C8 C9 C10 -1.1(4) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C9 C10 C11 C12 0.8(4) . . . . ? C10 C11 C12 C7 -0.7(4) . . . . ? C8 C7 C12 C11 -0.3(3) . . . . ? P1 C7 C12 C11 179.54(18) . . . . ? C7 P1 C13 C14 5.3(2) . . . . ? C1 P1 C13 C14 -105.20(19) . . . . ? Pd1 P1 C13 C14 125.00(17) . . . . ? C7 P1 C13 C18 -172.17(17) . . . . ? C1 P1 C13 C18 77.37(18) . . . . ? Pd1 P1 C13 C18 -52.43(18) . . . . ? C18 C13 C14 C15 -0.4(3) . . . . ? P1 C13 C14 C15 -177.81(18) . . . . ? C13 C14 C15 C16 -1.1(4) . . . . ? C14 C15 C16 C17 1.0(4) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? C16 C17 C18 C13 -2.2(4) . . . . ? C14 C13 C18 C17 2.1(3) . . . . ? P1 C13 C18 C17 179.63(18) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 33.36 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.857 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.162 ###END data_2#O_es _database_code_depnum_ccdc_archive 'CCDC 866982' #TrackingRef '- all_1_4_cif.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis-(Triphenylphosphine)dinitro-palladium(II) ; _chemical_formula_moiety 'C38 H34 Cl4 N2 O4 P2 Pd' _chemical_formula_sum 'C38 H34 Cl4 N2 O4 P2 Pd' _chemical_formula_weight 892.81 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.629(10) _cell_length_b 7.985(4) _cell_length_c 23.339(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3845(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9815 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 33.68 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9714 _exptl_absorpt_correction_T_max 0.9903 _exptl_absorpt_process_details ; SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline 13.3.1, ALS' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 38812 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 33.79 _reflns_number_total 5879 _reflns_number_gt 4771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+1.3680P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5879 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1089 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1184 0.1127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.7856 1.1793 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.0000 0.5000 0.0000 0.02072(7) Uani 1 2 d S . . Cl21 Cl -0.14748(4) 0.14118(9) 0.27527(3) 0.05343(17) Uani 1 1 d . . . Cl22 Cl -0.26773(4) 0.26059(10) 0.32790(3) 0.05961(19) Uani 1 1 d . . . P1 P 0.06427(2) 0.64919(5) -0.065747(18) 0.01962(10) Uani 1 1 d . A . O1 O -0.05616(15) 0.3614(4) -0.09858(17) 0.0315(9) Uani 0.540(9) 1 d P A 1 O2 O -0.1191(5) 0.5416(12) -0.0593(4) 0.0328(13) Uani 0.540(9) 1 d P A 1 N1 N -0.06775(19) 0.4665(5) -0.05958(15) 0.0217(9) Uani 0.540(9) 1 d P A 1 C1 C 0.02203(8) 0.7729(2) -0.12043(7) 0.0229(3) Uani 1 1 d . . . C2 C -0.01426(10) 0.6896(3) -0.16280(8) 0.0298(4) Uani 1 1 d . A . H2 H -0.0164 0.5707 -0.1630 0.036 Uiso 1 1 calc R . . C3 C -0.04698(10) 0.7815(3) -0.20439(9) 0.0351(4) Uani 1 1 d . . . H3 H -0.0718 0.7249 -0.2327 0.042 Uiso 1 1 calc R A . C4 C -0.04362(11) 0.9552(3) -0.20486(9) 0.0381(5) Uani 1 1 d . A . H4 H -0.0658 1.0169 -0.2336 0.046 Uiso 1 1 calc R . . C5 C -0.00800(11) 1.0386(3) -0.16337(11) 0.0376(5) Uani 1 1 d . . . H5 H -0.0058 1.1574 -0.1637 0.045 Uiso 1 1 calc R A . C6 C 0.02476(10) 0.9481(2) -0.12100(8) 0.0288(4) Uani 1 1 d . A . H6 H 0.0490 1.0057 -0.0925 0.035 Uiso 1 1 calc R . . C7 C 0.11430(9) 0.50519(19) -0.10703(8) 0.0217(3) Uani 1 1 d . . . C8 C 0.14403(9) 0.5577(2) -0.15808(8) 0.0276(3) Uani 1 1 d . A . H8 H 0.1387 0.6698 -0.1709 0.033 Uiso 1 1 calc R . . C9 C 0.18128(9) 0.4462(3) -0.18995(9) 0.0305(4) Uani 1 1 d . . . H9 H 0.2011 0.4819 -0.2246 0.037 Uiso 1 1 calc R A . C10 C 0.18954(9) 0.2815(3) -0.17090(9) 0.0306(4) Uani 1 1 d . A . H10 H 0.2149 0.2053 -0.1927 0.037 Uiso 1 1 calc R . . C11 C 0.16083(10) 0.2294(2) -0.12022(9) 0.0323(4) Uani 1 1 d . . . H11 H 0.1669 0.1177 -0.1072 0.039 Uiso 1 1 calc R A . C12 C 0.12294(9) 0.3402(2) -0.08816(8) 0.0272(3) Uani 1 1 d . A . H12 H 0.1031 0.3037 -0.0536 0.033 Uiso 1 1 calc R . . C13 C 0.11839(8) 0.7958(2) -0.02954(7) 0.0209(3) Uani 1 1 d . . . C14 C 0.18537(8) 0.7972(2) -0.03860(8) 0.0255(3) Uani 1 1 d . A . H14 H 0.2044 0.7230 -0.0656 0.031 Uiso 1 1 calc R . . C15 C 0.22420(10) 0.9088(3) -0.00751(9) 0.0309(4) Uani 1 1 d . . . H15 H 0.2698 0.9087 -0.0131 0.037 Uiso 1 1 calc R A . C16 C 0.19666(11) 1.0198(2) 0.03139(10) 0.0319(4) Uani 1 1 d . A . H16 H 0.2234 1.0956 0.0520 0.038 Uiso 1 1 calc R . . C17 C 0.12973(11) 1.0199(2) 0.04008(9) 0.0297(4) Uani 1 1 d . . . H17 H 0.1107 1.0969 0.0662 0.036 Uiso 1 1 calc R A . C18 C 0.09087(9) 0.9064(2) 0.01035(8) 0.0252(3) Uani 1 1 d . A . H18 H 0.0455 0.9040 0.0171 0.030 Uiso 1 1 calc R . . C21 C -0.18479(16) 0.2218(5) 0.33722(12) 0.0687(9) Uani 1 1 d . . . H21A H -0.1790 0.1411 0.3690 0.082 Uiso 1 1 calc R . . H21B H -0.1630 0.3274 0.3482 0.082 Uiso 1 1 calc R . . N1A N -0.1072(3) 0.4664(8) -0.0781(3) 0.0451(16) Uani 0.460(9) 1 d P A 2 O1A O -0.0490(2) 0.4060(6) -0.0714(2) 0.0350(12) Uani 0.460(9) 1 d P A 2 O2A O -0.1252(7) 0.5693(18) -0.0445(5) 0.045(2) Uani 0.460(9) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01441(11) 0.02587(12) 0.02186(11) 0.00305(6) -0.00168(6) -0.00390(6) Cl21 0.0671(4) 0.0527(4) 0.0405(3) 0.0103(3) 0.0014(3) -0.0084(3) Cl22 0.0634(4) 0.0617(4) 0.0537(4) -0.0009(3) -0.0174(3) 0.0152(3) P1 0.01402(18) 0.02200(19) 0.02285(19) 0.00139(15) 0.00038(14) -0.00105(14) O1 0.0355(16) 0.0340(15) 0.0249(17) -0.0087(12) -0.0037(12) -0.0039(11) O2 0.023(3) 0.040(3) 0.036(4) -0.002(2) -0.007(3) 0.004(2) N1 0.020(2) 0.0258(17) 0.0196(16) 0.0011(12) -0.0048(13) -0.0056(12) C1 0.0156(7) 0.0282(8) 0.0248(8) 0.0033(6) 0.0021(6) 0.0010(6) C2 0.0254(9) 0.0345(10) 0.0293(9) 0.0027(7) -0.0031(7) -0.0006(7) C3 0.0277(10) 0.0480(12) 0.0297(9) 0.0043(8) -0.0067(7) 0.0004(8) C4 0.0307(10) 0.0501(12) 0.0334(10) 0.0089(9) -0.0039(8) 0.0128(9) C5 0.0411(12) 0.0343(10) 0.0375(12) 0.0072(9) -0.0021(9) 0.0092(9) C6 0.0263(9) 0.0284(9) 0.0315(9) 0.0032(7) -0.0002(7) 0.0041(7) C7 0.0171(8) 0.0233(8) 0.0248(8) -0.0007(5) -0.0009(6) -0.0009(5) C8 0.0254(8) 0.0280(9) 0.0295(9) 0.0012(7) 0.0036(7) -0.0001(7) C9 0.0227(8) 0.0379(10) 0.0311(9) -0.0026(8) 0.0044(7) 0.0013(7) C10 0.0222(9) 0.0337(9) 0.0358(9) -0.0075(7) 0.0000(7) 0.0051(7) C11 0.0278(9) 0.0267(9) 0.0424(11) -0.0003(8) 0.0001(8) 0.0060(7) C12 0.0255(8) 0.0254(8) 0.0306(9) 0.0032(7) 0.0015(7) 0.0012(6) C13 0.0157(7) 0.0211(7) 0.0259(8) 0.0025(6) -0.0007(6) -0.0006(5) C14 0.0154(7) 0.0264(8) 0.0348(9) 0.0017(7) 0.0002(6) -0.0016(6) C15 0.0185(8) 0.0319(9) 0.0424(10) 0.0012(8) -0.0027(7) -0.0054(7) C16 0.0296(10) 0.0310(9) 0.0351(10) 0.0002(7) -0.0052(8) -0.0094(7) C17 0.0320(10) 0.0261(8) 0.0311(9) -0.0013(7) -0.0016(8) -0.0014(7) C18 0.0191(8) 0.0251(8) 0.0314(8) -0.0002(7) 0.0014(6) 0.0006(6) C21 0.0586(19) 0.108(3) 0.0393(14) -0.0114(15) -0.0121(13) 0.0010(18) N1A 0.037(3) 0.059(4) 0.039(3) 0.010(2) -0.008(2) -0.011(3) O1A 0.032(2) 0.040(3) 0.034(3) 0.002(2) -0.0018(17) -0.0129(18) O2A 0.024(2) 0.059(5) 0.051(6) 0.008(4) -0.003(4) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 1.990(3) . ? Pd1 N1 1.990(3) 5_565 ? Pd1 O1A 2.088(5) . ? Pd1 O1A 2.088(5) 5_565 ? Pd1 P1 2.3519(8) . ? Pd1 P1 2.3519(8) 5_565 ? Cl21 C21 1.760(3) . ? Cl22 C21 1.752(4) . ? P1 C7 1.8208(19) . ? P1 C13 1.8252(18) . ? P1 C1 1.8341(18) . ? O1 N1 1.261(5) . ? O2 N1 1.217(10) . ? C1 C6 1.400(3) . ? C1 C2 1.408(3) . ? C2 C3 1.391(3) . ? C2 H2 0.9500 . ? C3 C4 1.389(4) . ? C3 H3 0.9500 . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.399(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.400(2) . ? C7 C8 1.404(3) . ? C8 C9 1.392(3) . ? C8 H8 0.9500 . ? C9 C10 1.398(3) . ? C9 H9 0.9500 . ? C10 C11 1.387(3) . ? C10 H10 0.9500 . ? C11 C12 1.398(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.398(2) . ? C13 C18 1.403(2) . ? C14 C15 1.401(3) . ? C14 H14 0.9500 . ? C15 C16 1.390(3) . ? C15 H15 0.9500 . ? C16 C17 1.396(3) . ? C16 H16 0.9500 . ? C17 C18 1.395(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? N1A O2A 1.195(10) . ? N1A O1A 1.304(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.0(2) . 5_565 ? N1 Pd1 O1A 18.94(12) . . ? N1 Pd1 O1A 161.06(12) 5_565 . ? N1 Pd1 O1A 161.06(12) . 5_565 ? N1 Pd1 O1A 18.94(12) 5_565 5_565 ? O1A Pd1 O1A 180.00(17) . 5_565 ? N1 Pd1 P1 90.46(11) . . ? N1 Pd1 P1 89.54(11) 5_565 . ? O1A Pd1 P1 86.25(11) . . ? O1A Pd1 P1 93.75(11) 5_565 . ? N1 Pd1 P1 89.54(11) . 5_565 ? N1 Pd1 P1 90.46(11) 5_565 5_565 ? O1A Pd1 P1 93.75(11) . 5_565 ? O1A Pd1 P1 86.25(11) 5_565 5_565 ? P1 Pd1 P1 180.00(2) . 5_565 ? C7 P1 C13 107.66(9) . . ? C7 P1 C1 103.96(9) . . ? C13 P1 C1 105.50(9) . . ? C7 P1 Pd1 110.17(7) . . ? C13 P1 Pd1 111.57(6) . . ? C1 P1 Pd1 117.32(6) . . ? O2 N1 O1 119.8(5) . . ? O2 N1 Pd1 122.8(4) . . ? O1 N1 Pd1 117.4(3) . . ? C6 C1 C2 119.15(17) . . ? C6 C1 P1 121.71(14) . . ? C2 C1 P1 119.14(14) . . ? C3 C2 C1 119.93(19) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.5(2) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 120.1(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.1(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.2(2) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 119.48(17) . . ? C12 C7 P1 119.99(14) . . ? C8 C7 P1 120.53(13) . . ? C9 C8 C7 120.24(18) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.94(18) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.09(18) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.33(18) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 119.92(18) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C18 119.69(16) . . ? C14 C13 P1 122.66(14) . . ? C18 C13 P1 117.61(13) . . ? C13 C14 C15 119.46(18) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.69(19) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 119.95(18) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 119.76(19) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C13 120.42(18) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? Cl22 C21 Cl21 112.94(16) . . ? Cl22 C21 H21A 109.0 . . ? Cl21 C21 H21A 109.0 . . ? Cl22 C21 H21B 109.0 . . ? Cl21 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? O2A N1A O1A 117.5(10) . . ? N1A O1A Pd1 114.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 P1 C7 -86.38(14) . . . . ? N1 Pd1 P1 C7 93.62(14) 5_565 . . . ? O1A Pd1 P1 C7 -67.91(17) . . . . ? O1A Pd1 P1 C7 112.09(17) 5_565 . . . ? P1 Pd1 P1 C7 -146(100) 5_565 . . . ? N1 Pd1 P1 C13 154.09(14) . . . . ? N1 Pd1 P1 C13 -25.91(14) 5_565 . . . ? O1A Pd1 P1 C13 172.57(16) . . . . ? O1A Pd1 P1 C13 -7.43(16) 5_565 . . . ? P1 Pd1 P1 C13 95(100) 5_565 . . . ? N1 Pd1 P1 C1 32.25(14) . . . . ? N1 Pd1 P1 C1 -147.75(14) 5_565 . . . ? O1A Pd1 P1 C1 50.72(17) . . . . ? O1A Pd1 P1 C1 -129.28(17) 5_565 . . . ? P1 Pd1 P1 C1 -27(100) 5_565 . . . ? N1 Pd1 N1 O2 -112(100) 5_565 . . . ? O1A Pd1 N1 O2 176.4(10) . . . . ? O1A Pd1 N1 O2 -3.6(10) 5_565 . . . ? P1 Pd1 N1 O2 -106.6(7) . . . . ? P1 Pd1 N1 O2 73.4(7) 5_565 . . . ? N1 Pd1 N1 O1 68(100) 5_565 . . . ? O1A Pd1 N1 O1 -3.0(4) . . . . ? O1A Pd1 N1 O1 177.0(4) 5_565 . . . ? P1 Pd1 N1 O1 74.0(3) . . . . ? P1 Pd1 N1 O1 -106.0(3) 5_565 . . . ? C7 P1 C1 C6 -125.23(15) . . . . ? C13 P1 C1 C6 -12.07(17) . . . . ? Pd1 P1 C1 C6 112.87(14) . . . . ? C7 P1 C1 C2 54.99(16) . . . . ? C13 P1 C1 C2 168.15(14) . . . . ? Pd1 P1 C1 C2 -66.91(16) . . . . ? C6 C1 C2 C3 -0.2(3) . . . . ? P1 C1 C2 C3 179.56(15) . . . . ? C1 C2 C3 C4 0.7(3) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C3 C4 C5 C6 0.1(3) . . . . ? C4 C5 C6 C1 0.3(3) . . . . ? C2 C1 C6 C5 -0.3(3) . . . . ? P1 C1 C6 C5 179.95(16) . . . . ? C13 P1 C7 C12 106.06(16) . . . . ? C1 P1 C7 C12 -142.34(15) . . . . ? Pd1 P1 C7 C12 -15.81(17) . . . . ? C13 P1 C7 C8 -74.45(17) . . . . ? C1 P1 C7 C8 37.15(17) . . . . ? Pd1 P1 C7 C8 163.67(14) . . . . ? C12 C7 C8 C9 0.6(3) . . . . ? P1 C7 C8 C9 -178.87(15) . . . . ? C7 C8 C9 C10 -0.5(3) . . . . ? C8 C9 C10 C11 -0.2(3) . . . . ? C9 C10 C11 C12 0.7(3) . . . . ? C10 C11 C12 C7 -0.5(3) . . . . ? C8 C7 C12 C11 -0.1(3) . . . . ? P1 C7 C12 C11 179.35(15) . . . . ? C7 P1 C13 C14 5.11(17) . . . . ? C1 P1 C13 C14 -105.44(16) . . . . ? Pd1 P1 C13 C14 126.11(14) . . . . ? C7 P1 C13 C18 -172.54(14) . . . . ? C1 P1 C13 C18 76.91(15) . . . . ? Pd1 P1 C13 C18 -51.54(15) . . . . ? C18 C13 C14 C15 0.2(3) . . . . ? P1 C13 C14 C15 -177.39(14) . . . . ? C13 C14 C15 C16 -1.1(3) . . . . ? C14 C15 C16 C17 0.5(3) . . . . ? C15 C16 C17 C18 1.1(3) . . . . ? C16 C17 C18 C13 -2.0(3) . . . . ? C14 C13 C18 C17 1.3(3) . . . . ? P1 C13 C18 C17 179.06(14) . . . . ? O2A N1A O1A Pd1 1.7(12) . . . . ? N1 Pd1 O1A N1A -5.4(4) . . . . ? N1 Pd1 O1A N1A 174.6(4) 5_565 . . . ? O1A Pd1 O1A N1A 90(100) 5_565 . . . ? P1 Pd1 O1A N1A -107.9(4) . . . . ? P1 Pd1 O1A N1A 72.1(4) 5_565 . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 33.79 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.269 _refine_diff_density_min -1.740 _refine_diff_density_rms 0.108 ###END data_3_gs _database_code_depnum_ccdc_archive 'CCDC 866983' #TrackingRef '- all_1_4_cif.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis-(Triphenylarsine)dinitro-palladium(II) ; _chemical_formula_moiety 'C36 H30 As2 N2 O4 Pd' _chemical_formula_sum 'C36 H30 As2 N2 O4 Pd' _chemical_formula_weight 810.86 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5940(7) _cell_length_b 9.9987(7) _cell_length_c 10.1274(7) _cell_angle_alpha 111.490(1) _cell_angle_beta 90.473(1) _cell_angle_gamma 115.209(1) _cell_volume 802.14(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6896 _cell_measurement_theta_min 4.02 _cell_measurement_theta_max 33.59 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 3.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8550 _exptl_absorpt_correction_T_max 0.9684 _exptl_absorpt_process_details ; SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline 13.3.1, ALS' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10978 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 33.59 _reflns_number_total 4729 _reflns_number_gt 4310 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4729 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1621 _refine_ls_wR_factor_gt 0.1589 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.7856 1.1793 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As -0.1496 2.3280 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.5000 0.5000 0.5000 0.01547(12) Uani 1 2 d S . . As1 As 0.52346(3) 0.73334(3) 0.71038(3) 0.01472(12) Uani 1 1 d . . . O1 O 0.7017(3) 0.6771(3) 0.3572(3) 0.0312(5) Uani 1 1 d . . . O2 O 0.8279(3) 0.6968(3) 0.5463(3) 0.0312(5) Uani 1 1 d . . . N1 N 0.7057(3) 0.6435(3) 0.4613(3) 0.0217(5) Uani 1 1 d . . . C1 C 0.5945(3) 0.9388(3) 0.6944(3) 0.0177(5) Uani 1 1 d . . . C2 C 0.7400(3) 1.0086(3) 0.6561(3) 0.0209(5) Uani 1 1 d . . . H2 H 0.8060 0.9578 0.6417 0.025 Uiso 1 1 calc R . . C3 C 0.7872(4) 1.1523(4) 0.6391(3) 0.0248(6) Uani 1 1 d . . . H3 H 0.8863 1.2007 0.6142 0.030 Uiso 1 1 calc R . . C4 C 0.6888(4) 1.2260(4) 0.6586(3) 0.0249(6) Uani 1 1 d . . . H4 H 0.7210 1.3238 0.6460 0.030 Uiso 1 1 calc R . . C5 C 0.5452(4) 1.1574(3) 0.6961(3) 0.0232(5) Uani 1 1 d . . . H5 H 0.4793 1.2082 0.7095 0.028 Uiso 1 1 calc R . . C6 C 0.4966(3) 1.0129(3) 0.7146(3) 0.0200(5) Uani 1 1 d . . . H6 H 0.3980 0.9656 0.7405 0.024 Uiso 1 1 calc R . . C7 C 0.6582(3) 0.7740(3) 0.8777(3) 0.0164(5) Uani 1 1 d . . . C8 C 0.7649(3) 0.9304(3) 0.9729(3) 0.0216(5) Uani 1 1 d . . . H8 H 0.7797 1.0201 0.9519 0.026 Uiso 1 1 calc R . . C9 C 0.8501(3) 0.9550(4) 1.0995(3) 0.0238(6) Uani 1 1 d . . . H9 H 0.9240 1.0614 1.1641 0.029 Uiso 1 1 calc R . . C10 C 0.8263(3) 0.8231(4) 1.1306(3) 0.0244(6) Uani 1 1 d . . . H10 H 0.8826 0.8398 1.2176 0.029 Uiso 1 1 calc R . . C11 C 0.7208(3) 0.6673(4) 1.0348(3) 0.0229(5) Uani 1 1 d . . . H11 H 0.7054 0.5776 1.0563 0.027 Uiso 1 1 calc R . . C12 C 0.6377(3) 0.6420(3) 0.9076(3) 0.0203(5) Uani 1 1 d . . . H12 H 0.5671 0.5351 0.8412 0.024 Uiso 1 1 calc R . . C13 C 0.3255(3) 0.6937(3) 0.7739(3) 0.0167(5) Uani 1 1 d . . . C14 C 0.3095(3) 0.7002(3) 0.9125(3) 0.0182(5) Uani 1 1 d . . . H14 H 0.3980 0.7302 0.9800 0.022 Uiso 1 1 calc R . . C15 C 0.1625(3) 0.6625(4) 0.9517(3) 0.0219(5) Uani 1 1 d . . . H15 H 0.1509 0.6664 1.0459 0.026 Uiso 1 1 calc R . . C16 C 0.0336(3) 0.6192(4) 0.8527(3) 0.0234(5) Uani 1 1 d . . . H16 H -0.0667 0.5914 0.8789 0.028 Uiso 1 1 calc R . . C17 C 0.0504(3) 0.6162(4) 0.7157(3) 0.0234(5) Uani 1 1 d . . . H17 H -0.0375 0.5902 0.6495 0.028 Uiso 1 1 calc R . . C18 C 0.1950(3) 0.6512(3) 0.6755(3) 0.0202(5) Uani 1 1 d . . . H18 H 0.2058 0.6464 0.5809 0.024 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01874(18) 0.01371(17) 0.01381(17) 0.00525(12) 0.00513(12) 0.00762(13) As1 0.01760(18) 0.01325(17) 0.01302(17) 0.00493(12) 0.00378(11) 0.00721(13) O1 0.0400(13) 0.0297(12) 0.0262(11) 0.0167(10) 0.0118(10) 0.0136(10) O2 0.0246(11) 0.0291(12) 0.0378(13) 0.0135(10) 0.0013(9) 0.0109(9) N1 0.0280(12) 0.0180(11) 0.0221(11) 0.0061(9) 0.0061(9) 0.0148(10) C1 0.0238(12) 0.0150(11) 0.0139(11) 0.0052(9) 0.0024(9) 0.0093(10) C2 0.0215(12) 0.0196(12) 0.0199(12) 0.0082(10) 0.0059(10) 0.0077(10) C3 0.0268(14) 0.0219(13) 0.0199(13) 0.0097(11) 0.0039(11) 0.0053(11) C4 0.0331(15) 0.0179(12) 0.0195(13) 0.0091(10) 0.0009(11) 0.0071(11) C5 0.0302(14) 0.0178(12) 0.0218(13) 0.0083(10) 0.0012(11) 0.0112(11) C6 0.0233(12) 0.0178(12) 0.0176(12) 0.0066(10) 0.0024(10) 0.0090(10) C7 0.0196(11) 0.0170(11) 0.0141(11) 0.0069(9) 0.0036(9) 0.0093(9) C8 0.0250(13) 0.0177(12) 0.0217(13) 0.0077(10) 0.0029(10) 0.0097(10) C9 0.0233(13) 0.0230(13) 0.0192(13) 0.0065(11) 0.0005(10) 0.0075(11) C10 0.0231(13) 0.0325(15) 0.0240(13) 0.0158(12) 0.0069(11) 0.0148(12) C11 0.0244(13) 0.0264(14) 0.0288(14) 0.0179(12) 0.0083(11) 0.0154(11) C12 0.0210(12) 0.0182(12) 0.0239(13) 0.0096(10) 0.0049(10) 0.0100(10) C13 0.0179(11) 0.0130(11) 0.0169(11) 0.0038(9) 0.0029(9) 0.0071(9) C14 0.0206(12) 0.0177(11) 0.0159(11) 0.0058(9) 0.0045(9) 0.0095(10) C15 0.0246(13) 0.0229(13) 0.0208(12) 0.0100(10) 0.0088(10) 0.0122(11) C16 0.0217(13) 0.0188(12) 0.0265(14) 0.0070(11) 0.0063(11) 0.0086(10) C17 0.0172(12) 0.0226(13) 0.0264(14) 0.0084(11) -0.0007(10) 0.0073(10) C18 0.0218(12) 0.0218(13) 0.0182(12) 0.0088(10) 0.0023(10) 0.0107(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.029(3) . ? Pd1 N1 2.029(3) 2_666 ? Pd1 As1 2.4364(3) 2_666 ? Pd1 As1 2.4364(3) . ? As1 C7 1.928(3) . ? As1 C13 1.935(3) . ? As1 C1 1.941(3) . ? O1 N1 1.223(3) . ? O2 N1 1.231(3) . ? C1 C6 1.399(4) . ? C1 C2 1.401(4) . ? C2 C3 1.389(4) . ? C2 H2 0.9500 . ? C3 C4 1.401(5) . ? C3 H3 0.9500 . ? C4 C5 1.381(4) . ? C4 H4 0.9500 . ? C5 C6 1.402(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.392(4) . ? C7 C12 1.395(4) . ? C8 C9 1.397(4) . ? C8 H8 0.9500 . ? C9 C10 1.393(4) . ? C9 H9 0.9500 . ? C10 C11 1.387(4) . ? C10 H10 0.9500 . ? C11 C12 1.390(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.394(4) . ? C13 C18 1.399(4) . ? C14 C15 1.397(4) . ? C14 H14 0.9500 . ? C15 C16 1.388(4) . ? C15 H15 0.9500 . ? C16 C17 1.390(4) . ? C16 H16 0.9500 . ? C17 C18 1.383(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.0(2) . 2_666 ? N1 Pd1 As1 90.47(7) . 2_666 ? N1 Pd1 As1 89.53(7) 2_666 2_666 ? N1 Pd1 As1 89.53(7) . . ? N1 Pd1 As1 90.47(7) 2_666 . ? As1 Pd1 As1 180.0 2_666 . ? C7 As1 C13 102.51(11) . . ? C7 As1 C1 106.55(11) . . ? C13 As1 C1 104.66(11) . . ? C7 As1 Pd1 111.67(8) . . ? C13 As1 Pd1 111.61(8) . . ? C1 As1 Pd1 118.43(8) . . ? O1 N1 O2 123.1(3) . . ? O1 N1 Pd1 118.4(2) . . ? O2 N1 Pd1 118.5(2) . . ? C6 C1 C2 120.3(3) . . ? C6 C1 As1 119.6(2) . . ? C2 C1 As1 120.0(2) . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 119.5(3) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C8 C7 C12 120.1(2) . . ? C8 C7 As1 121.8(2) . . ? C12 C7 As1 117.9(2) . . ? C7 C8 C9 119.8(3) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 119.8(3) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C14 C13 C18 119.9(2) . . ? C14 C13 As1 121.5(2) . . ? C18 C13 As1 118.6(2) . . ? C13 C14 C15 119.7(2) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.3(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.1(3) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 As1 C7 -82.56(11) . . . . ? N1 Pd1 As1 C7 97.44(11) 2_666 . . . ? As1 Pd1 As1 C7 0(100) 2_666 . . . ? N1 Pd1 As1 C13 163.36(11) . . . . ? N1 Pd1 As1 C13 -16.64(11) 2_666 . . . ? As1 Pd1 As1 C13 0(100) 2_666 . . . ? N1 Pd1 As1 C1 41.76(12) . . . . ? N1 Pd1 As1 C1 -138.24(12) 2_666 . . . ? As1 Pd1 As1 C1 0(100) 2_666 . . . ? N1 Pd1 N1 O1 -45(100) 2_666 . . . ? As1 Pd1 N1 O1 71.4(2) 2_666 . . . ? As1 Pd1 N1 O1 -108.6(2) . . . . ? N1 Pd1 N1 O2 133(100) 2_666 . . . ? As1 Pd1 N1 O2 -110.9(2) 2_666 . . . ? As1 Pd1 N1 O2 69.1(2) . . . . ? C7 As1 C1 C6 -113.9(2) . . . . ? C13 As1 C1 C6 -5.8(2) . . . . ? Pd1 As1 C1 C6 119.30(19) . . . . ? C7 As1 C1 C2 69.1(2) . . . . ? C13 As1 C1 C2 177.3(2) . . . . ? Pd1 As1 C1 C2 -57.7(2) . . . . ? C6 C1 C2 C3 0.4(4) . . . . ? As1 C1 C2 C3 177.4(2) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? C3 C4 C5 C6 -0.2(4) . . . . ? C2 C1 C6 C5 0.0(4) . . . . ? As1 C1 C6 C5 -177.0(2) . . . . ? C4 C5 C6 C1 -0.1(4) . . . . ? C13 As1 C7 C8 -100.8(2) . . . . ? C1 As1 C7 C8 8.9(3) . . . . ? Pd1 As1 C7 C8 139.6(2) . . . . ? C13 As1 C7 C12 74.4(2) . . . . ? C1 As1 C7 C12 -175.9(2) . . . . ? Pd1 As1 C7 C12 -45.2(2) . . . . ? C12 C7 C8 C9 -0.8(4) . . . . ? As1 C7 C8 C9 174.3(2) . . . . ? C7 C8 C9 C10 -0.8(4) . . . . ? C8 C9 C10 C11 1.3(4) . . . . ? C9 C10 C11 C12 -0.3(4) . . . . ? C10 C11 C12 C7 -1.3(4) . . . . ? C8 C7 C12 C11 1.8(4) . . . . ? As1 C7 C12 C11 -173.5(2) . . . . ? C7 As1 C13 C14 0.5(2) . . . . ? C1 As1 C13 C14 -110.6(2) . . . . ? Pd1 As1 C13 C14 120.1(2) . . . . ? C7 As1 C13 C18 -176.9(2) . . . . ? C1 As1 C13 C18 72.0(2) . . . . ? Pd1 As1 C13 C18 -57.3(2) . . . . ? C18 C13 C14 C15 0.7(4) . . . . ? As1 C13 C14 C15 -176.6(2) . . . . ? C13 C14 C15 C16 -0.2(4) . . . . ? C14 C15 C16 C17 -1.3(4) . . . . ? C15 C16 C17 C18 2.2(4) . . . . ? C16 C17 C18 C13 -1.7(4) . . . . ? C14 C13 C18 C17 0.2(4) . . . . ? As1 C13 C18 C17 177.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 33.59 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.877 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.232 ###END data_3#O_es _database_code_depnum_ccdc_archive 'CCDC 866984' #TrackingRef '- all_1_4_cif.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis-(Triphenylarsine)dinitro-palladium(II) ; _chemical_formula_moiety 'C36 H30 As2 N2 O4 Pd' _chemical_formula_sum 'C36 H30 As2 N2 O4 Pd' _chemical_formula_weight 810.86 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5967(9) _cell_length_b 9.9479(9) _cell_length_c 10.1121(9) _cell_angle_alpha 111.262(1) _cell_angle_beta 90.931(1) _cell_angle_gamma 114.454(1) _cell_volume 803.05(13) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6896 _cell_measurement_theta_min 4.02 _cell_measurement_theta_max 33.59 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 3.234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8550 _exptl_absorpt_correction_T_max 0.9684 _exptl_absorpt_process_details ; SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Beamline 13.3.1, ALS' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11526 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 33.65 _reflns_number_total 4795 _reflns_number_gt 4301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.1223P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4795 _refine_ls_number_parameters 237 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.7856 1.1793 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As -0.1496 2.3280 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.5000 0.5000 0.5000 0.02180(8) Uani 1 2 d S . . As1 As 0.52110(2) 0.73229(2) 0.70973(2) 0.02080(8) Uani 1 1 d . A . O1 O 0.7114(8) 0.6695(9) 0.3586(8) 0.0448(13) Uani 0.600(3) 1 d P A 1 O2 O 0.8247(8) 0.6933(7) 0.5462(7) 0.0387(15) Uani 0.600(3) 1 d P A 1 N1 N 0.7024(4) 0.6422(4) 0.4633(4) 0.0292(8) Uani 0.600(3) 1 d P A 1 C1 C 0.5908(2) 0.9390(2) 0.6949(2) 0.0226(4) Uani 1 1 d . . . C2 C 0.7361(3) 1.0083(3) 0.6589(2) 0.0279(4) Uani 1 1 d . A . H2 H 0.8023 0.9571 0.6454 0.033 Uiso 1 1 calc R . . C3 C 0.7830(3) 1.1536(3) 0.6431(3) 0.0322(5) Uani 1 1 d . . . H3 H 0.8819 1.2020 0.6195 0.039 Uiso 1 1 calc R A . C4 C 0.6851(3) 1.2274(3) 0.6618(3) 0.0324(5) Uani 1 1 d . A . H4 H 0.7174 1.3261 0.6507 0.039 Uiso 1 1 calc R . . C5 C 0.5409(3) 1.1579(3) 0.6965(2) 0.0296(5) Uani 1 1 d . . . H5 H 0.4742 1.2085 0.7082 0.036 Uiso 1 1 calc R A . C6 C 0.4935(3) 1.0139(3) 0.7142(2) 0.0257(4) Uani 1 1 d . A . H6 H 0.3952 0.9669 0.7394 0.031 Uiso 1 1 calc R . . C7 C 0.6554(2) 0.7720(3) 0.8777(2) 0.0226(4) Uani 1 1 d . . . C8 C 0.7625(3) 0.9277(3) 0.9723(2) 0.0264(4) Uani 1 1 d . A . H8 H 0.7766 1.0177 0.9515 0.032 Uiso 1 1 calc R . . C9 C 0.8489(3) 0.9505(3) 1.0980(3) 0.0300(5) Uani 1 1 d . . . H9 H 0.9230 1.0562 1.1619 0.036 Uiso 1 1 calc R A . C10 C 0.8268(3) 0.8196(3) 1.1295(3) 0.0310(5) Uani 1 1 d . A . H10 H 0.8844 0.8357 1.2157 0.037 Uiso 1 1 calc R . . C11 C 0.7200(3) 0.6645(3) 1.0346(3) 0.0319(5) Uani 1 1 d . . . H11 H 0.7046 0.5749 1.0567 0.038 Uiso 1 1 calc R A . C12 C 0.6358(3) 0.6398(3) 0.9081(3) 0.0286(4) Uani 1 1 d . A . H12 H 0.5652 0.5334 0.8424 0.034 Uiso 1 1 calc R . . C13 C 0.3241(2) 0.6945(2) 0.7724(2) 0.0216(4) Uani 1 1 d . . . C14 C 0.3066(3) 0.6999(3) 0.9102(2) 0.0239(4) Uani 1 1 d . A . H14 H 0.3944 0.7293 0.9785 0.029 Uiso 1 1 calc R . . C15 C 0.1608(3) 0.6622(3) 0.9482(3) 0.0289(4) Uani 1 1 d . . . H15 H 0.1489 0.6649 1.0421 0.035 Uiso 1 1 calc R A . C16 C 0.0331(3) 0.6208(3) 0.8494(3) 0.0320(5) Uani 1 1 d . A . H16 H -0.0667 0.5940 0.8751 0.038 Uiso 1 1 calc R . . C17 C 0.0508(3) 0.6185(3) 0.7124(3) 0.0316(5) Uani 1 1 d . . . H17 H -0.0364 0.5930 0.6457 0.038 Uiso 1 1 calc R A . C18 C 0.1946(3) 0.6529(3) 0.6731(2) 0.0271(4) Uani 1 1 d . A . H18 H 0.2056 0.6484 0.5786 0.033 Uiso 1 1 calc R . . O1A O 0.6241(14) 0.618(2) 0.3940(18) 0.0226(10) Uiso 0.124(5) 1 d PD A 3 N1A N 0.7790(15) 0.709(2) 0.4303(19) 0.0226(10) Uiso 0.124(5) 1 d PD A 3 O2A O 0.832(3) 0.719(4) 0.559(3) 0.0226(10) Uiso 0.124(5) 1 d PD A 3 O1B O 0.7336(11) 0.6244(10) 0.5353(9) 0.0226(10) Uiso 0.192(4) 1 d PD A 2 N1B N 0.7986(11) 0.6844(13) 0.4399(11) 0.0226(10) Uiso 0.192(4) 1 d PD A 2 O2B O 0.692(2) 0.685(2) 0.3561(19) 0.0226(10) Uiso 0.192(4) 1 d PD A 2 O1C O 0.635(2) 0.641(3) 0.380(3) 0.0226(10) Uiso 0.085(3) 1 d PD A 4 O2C O 0.8901(17) 0.767(2) 0.4276(19) 0.0226(10) Uiso 0.085(3) 1 d PD A 4 N1C N 0.763(2) 0.682(3) 0.471(2) 0.0226(10) Uiso 0.085(3) 1 d PD A 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02338(12) 0.01811(12) 0.02086(12) 0.00512(9) 0.00617(9) 0.00893(9) As1 0.02439(13) 0.01806(12) 0.01865(12) 0.00532(9) 0.00422(9) 0.01023(9) O1 0.059(4) 0.039(3) 0.050(2) 0.0264(19) 0.026(2) 0.027(2) O2 0.030(2) 0.028(3) 0.051(3) 0.009(2) -0.0015(15) 0.013(2) N1 0.0267(16) 0.0157(15) 0.0374(19) 0.0041(13) 0.0064(15) 0.0082(13) C1 0.0272(10) 0.0195(9) 0.0174(8) 0.0061(7) 0.0012(7) 0.0085(8) C2 0.0283(10) 0.0274(11) 0.0232(10) 0.0090(8) 0.0035(8) 0.0095(9) C3 0.0329(12) 0.0281(11) 0.0262(11) 0.0112(9) 0.0035(9) 0.0051(9) C4 0.0434(13) 0.0227(10) 0.0234(10) 0.0107(8) -0.0031(9) 0.0071(9) C5 0.0395(12) 0.0244(10) 0.0253(10) 0.0084(8) -0.0005(9) 0.0164(9) C6 0.0281(10) 0.0230(10) 0.0234(10) 0.0074(8) 0.0025(8) 0.0109(8) C7 0.0250(9) 0.0229(9) 0.0234(9) 0.0096(8) 0.0060(8) 0.0137(8) C8 0.0310(11) 0.0227(10) 0.0250(10) 0.0085(8) 0.0047(8) 0.0128(9) C9 0.0278(10) 0.0293(11) 0.0277(11) 0.0084(9) 0.0010(9) 0.0110(9) C10 0.0277(11) 0.0408(13) 0.0321(12) 0.0195(10) 0.0051(9) 0.0184(10) C11 0.0320(11) 0.0346(12) 0.0419(13) 0.0236(11) 0.0104(10) 0.0195(10) C12 0.0275(10) 0.0226(10) 0.0371(12) 0.0126(9) 0.0054(9) 0.0121(8) C13 0.0249(9) 0.0161(8) 0.0209(9) 0.0047(7) 0.0039(7) 0.0089(7) C14 0.0287(10) 0.0194(9) 0.0222(9) 0.0065(8) 0.0056(8) 0.0111(8) C15 0.0345(11) 0.0255(10) 0.0260(10) 0.0091(9) 0.0108(9) 0.0137(9) C16 0.0261(10) 0.0266(11) 0.0351(12) 0.0067(9) 0.0101(9) 0.0093(9) C17 0.0249(10) 0.0291(11) 0.0324(12) 0.0077(9) 0.0005(9) 0.0088(9) C18 0.0294(10) 0.0258(10) 0.0212(9) 0.0064(8) 0.0018(8) 0.0108(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 O1A 1.936(14) 2_666 ? Pd1 O1A 1.936(14) . ? Pd1 O1B 2.010(9) . ? Pd1 O1B 2.010(9) 2_666 ? Pd1 N1 2.010(4) 2_666 ? Pd1 N1 2.010(4) . ? Pd1 O1C 2.21(3) 2_666 ? Pd1 O1C 2.21(3) . ? Pd1 As1 2.4337(3) . ? Pd1 As1 2.4337(3) 2_666 ? Pd1 N1C 2.520(17) . ? Pd1 N1C 2.520(17) 2_666 ? As1 C7 1.929(2) . ? As1 C13 1.934(2) . ? As1 C1 1.946(2) . ? O1 N1 1.181(8) . ? O2 N1 1.225(7) . ? C1 C6 1.393(3) . ? C1 C2 1.397(3) . ? C2 C3 1.396(3) . ? C2 H2 0.9500 . ? C3 C4 1.391(4) . ? C3 H3 0.9500 . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.395(3) . ? C7 C12 1.397(3) . ? C8 C9 1.398(3) . ? C8 H8 0.9500 . ? C9 C10 1.385(3) . ? C9 H9 0.9500 . ? C10 C11 1.392(4) . ? C10 H10 0.9500 . ? C11 C12 1.387(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.391(3) . ? C13 C18 1.399(3) . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C16 1.384(3) . ? C15 H15 0.9500 . ? C16 C17 1.391(4) . ? C16 H16 0.9500 . ? C17 C18 1.380(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O1A N1A 1.338(9) . ? N1A O2A 1.343(9) . ? O1B N1B 1.344(8) . ? N1B O2B 1.321(8) . ? O1C N1C 1.342(10) . ? O2C N1C 1.355(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Pd1 O1A 180.000(3) 2_666 . ? O1A Pd1 O1B 128.1(4) 2_666 . ? O1A Pd1 O1B 51.9(4) . . ? O1A Pd1 O1B 51.9(4) 2_666 2_666 ? O1A Pd1 O1B 128.1(4) . 2_666 ? O1B Pd1 O1B 180.000(1) . 2_666 ? O1A Pd1 N1 26.6(4) 2_666 2_666 ? O1A Pd1 N1 153.4(4) . 2_666 ? O1B Pd1 N1 154.6(2) . 2_666 ? O1B Pd1 N1 25.4(2) 2_666 2_666 ? O1A Pd1 N1 153.4(4) 2_666 . ? O1A Pd1 N1 26.6(4) . . ? O1B Pd1 N1 25.4(2) . . ? O1B Pd1 N1 154.6(2) 2_666 . ? N1 Pd1 N1 180.00(17) 2_666 . ? O1A Pd1 O1C 2.8(10) 2_666 2_666 ? O1A Pd1 O1C 177.2(10) . 2_666 ? O1B Pd1 O1C 126.4(6) . 2_666 ? O1B Pd1 O1C 53.6(6) 2_666 2_666 ? N1 Pd1 O1C 28.2(5) 2_666 2_666 ? N1 Pd1 O1C 151.8(5) . 2_666 ? O1A Pd1 O1C 177.2(10) 2_666 . ? O1A Pd1 O1C 2.8(10) . . ? O1B Pd1 O1C 53.6(6) . . ? O1B Pd1 O1C 126.4(6) 2_666 . ? N1 Pd1 O1C 151.8(5) 2_666 . ? N1 Pd1 O1C 28.2(5) . . ? O1C Pd1 O1C 180.000(4) 2_666 . ? O1A Pd1 As1 82.7(5) 2_666 . ? O1A Pd1 As1 97.3(5) . . ? O1B Pd1 As1 84.2(2) . . ? O1B Pd1 As1 95.8(2) 2_666 . ? N1 Pd1 As1 90.65(10) 2_666 . ? N1 Pd1 As1 89.35(10) . . ? O1C Pd1 As1 84.5(7) 2_666 . ? O1C Pd1 As1 95.5(7) . . ? O1A Pd1 As1 97.3(5) 2_666 2_666 ? O1A Pd1 As1 82.7(5) . 2_666 ? O1B Pd1 As1 95.8(2) . 2_666 ? O1B Pd1 As1 84.2(2) 2_666 2_666 ? N1 Pd1 As1 89.35(10) 2_666 2_666 ? N1 Pd1 As1 90.65(10) . 2_666 ? O1C Pd1 As1 95.5(7) 2_666 2_666 ? O1C Pd1 As1 84.5(7) . 2_666 ? As1 Pd1 As1 180.0 . 2_666 ? O1A Pd1 N1C 149.5(7) 2_666 . ? O1A Pd1 N1C 30.5(7) . . ? O1B Pd1 N1C 21.6(6) . . ? O1B Pd1 N1C 158.4(6) 2_666 . ? N1 Pd1 N1C 176.0(5) 2_666 . ? N1 Pd1 N1C 4.0(5) . . ? O1C Pd1 N1C 147.9(3) 2_666 . ? O1C Pd1 N1C 32.1(3) . . ? As1 Pd1 N1C 87.4(7) . . ? As1 Pd1 N1C 92.6(7) 2_666 . ? O1A Pd1 N1C 30.5(7) 2_666 2_666 ? O1A Pd1 N1C 149.5(7) . 2_666 ? O1B Pd1 N1C 158.4(6) . 2_666 ? O1B Pd1 N1C 21.6(6) 2_666 2_666 ? N1 Pd1 N1C 4.0(5) 2_666 2_666 ? N1 Pd1 N1C 176.0(5) . 2_666 ? O1C Pd1 N1C 32.1(3) 2_666 2_666 ? O1C Pd1 N1C 147.9(3) . 2_666 ? As1 Pd1 N1C 92.6(7) . 2_666 ? As1 Pd1 N1C 87.4(7) 2_666 2_666 ? N1C Pd1 N1C 180.000(2) . 2_666 ? C7 As1 C13 102.70(9) . . ? C7 As1 C1 106.20(9) . . ? C13 As1 C1 104.20(9) . . ? C7 As1 Pd1 111.65(6) . . ? C13 As1 Pd1 111.88(6) . . ? C1 As1 Pd1 118.75(6) . . ? O1 N1 O2 117.4(7) . . ? O1 N1 Pd1 122.9(5) . . ? O2 N1 Pd1 119.5(4) . . ? C6 C1 C2 120.3(2) . . ? C6 C1 As1 120.03(16) . . ? C2 C1 As1 119.59(17) . . ? C3 C2 C1 119.4(2) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C4 C3 C2 120.1(2) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.4(2) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.0(2) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 119.8(2) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C8 C7 C12 120.0(2) . . ? C8 C7 As1 122.04(16) . . ? C12 C7 As1 117.82(17) . . ? C7 C8 C9 119.7(2) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.2(2) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.9(2) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.5(2) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 119.7(2) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C14 C13 C18 119.6(2) . . ? C14 C13 As1 121.83(16) . . ? C18 C13 As1 118.54(16) . . ? C15 C14 C13 120.1(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.1(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.0(2) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.3(2) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C13 120.0(2) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? N1A O1A Pd1 125.0(11) . . ? O1A N1A O2A 109.5(13) . . ? N1B O1B Pd1 118.9(7) . . ? O2B N1B O1B 110.1(11) . . ? N1C O1C Pd1 86.8(13) . . ? O1C N1C O2C 108.5(13) . . ? O1C N1C Pd1 61.1(12) . . ? O2C N1C Pd1 168.5(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A Pd1 As1 C7 72.2(4) 2_666 . . . ? O1A Pd1 As1 C7 -107.8(4) . . . . ? O1B Pd1 As1 C7 -57.4(2) . . . . ? O1B Pd1 As1 C7 122.6(2) 2_666 . . . ? N1 Pd1 As1 C7 97.67(13) 2_666 . . . ? N1 Pd1 As1 C7 -82.33(13) . . . . ? O1C Pd1 As1 C7 70.1(5) 2_666 . . . ? O1C Pd1 As1 C7 -109.9(5) . . . . ? As1 Pd1 As1 C7 -170(92) 2_666 . . . ? N1C Pd1 As1 C7 -78.8(5) . . . . ? N1C Pd1 As1 C7 101.2(5) 2_666 . . . ? O1A Pd1 As1 C13 -42.2(4) 2_666 . . . ? O1A Pd1 As1 C13 137.8(4) . . . . ? O1B Pd1 As1 C13 -171.9(2) . . . . ? O1B Pd1 As1 C13 8.1(2) 2_666 . . . ? N1 Pd1 As1 C13 -16.81(13) 2_666 . . . ? N1 Pd1 As1 C13 163.19(13) . . . . ? O1C Pd1 As1 C13 -44.4(5) 2_666 . . . ? O1C Pd1 As1 C13 135.6(5) . . . . ? As1 Pd1 As1 C13 76(92) 2_666 . . . ? N1C Pd1 As1 C13 166.7(5) . . . . ? N1C Pd1 As1 C13 -13.3(5) 2_666 . . . ? O1A Pd1 As1 C1 -163.7(4) 2_666 . . . ? O1A Pd1 As1 C1 16.3(4) . . . . ? O1B Pd1 As1 C1 66.7(2) . . . . ? O1B Pd1 As1 C1 -113.3(2) 2_666 . . . ? N1 Pd1 As1 C1 -138.27(13) 2_666 . . . ? N1 Pd1 As1 C1 41.73(13) . . . . ? O1C Pd1 As1 C1 -165.9(5) 2_666 . . . ? O1C Pd1 As1 C1 14.1(5) . . . . ? As1 Pd1 As1 C1 -46(92) 2_666 . . . ? N1C Pd1 As1 C1 45.3(5) . . . . ? N1C Pd1 As1 C1 -134.7(5) 2_666 . . . ? O1A Pd1 N1 O1 172.2(13) 2_666 . . . ? O1A Pd1 N1 O1 -7.8(13) . . . . ? O1B Pd1 N1 O1 166.6(8) . . . . ? O1B Pd1 N1 O1 -13.4(8) 2_666 . . . ? N1 Pd1 N1 O1 -13(100) 2_666 . . . ? O1C Pd1 N1 O1 167.4(16) 2_666 . . . ? O1C Pd1 N1 O1 -12.6(16) . . . . ? As1 Pd1 N1 O1 -115.6(4) . . . . ? As1 Pd1 N1 O1 64.4(4) 2_666 . . . ? N1C Pd1 N1 O1 -177(10) . . . . ? N1C Pd1 N1 O1 3(10) 2_666 . . . ? O1A Pd1 N1 O2 -1.9(13) 2_666 . . . ? O1A Pd1 N1 O2 178.1(13) . . . . ? O1B Pd1 N1 O2 -7.4(7) . . . . ? O1B Pd1 N1 O2 172.6(7) 2_666 . . . ? N1 Pd1 N1 O2 173(100) 2_666 . . . ? O1C Pd1 N1 O2 -6.7(17) 2_666 . . . ? O1C Pd1 N1 O2 173.3(17) . . . . ? As1 Pd1 N1 O2 70.4(4) . . . . ? As1 Pd1 N1 O2 -109.6(4) 2_666 . . . ? N1C Pd1 N1 O2 9(10) . . . . ? N1C Pd1 N1 O2 -171(10) 2_666 . . . ? C7 As1 C1 C6 -114.09(17) . . . . ? C13 As1 C1 C6 -6.05(19) . . . . ? Pd1 As1 C1 C6 119.22(16) . . . . ? C7 As1 C1 C2 68.52(18) . . . . ? C13 As1 C1 C2 176.56(16) . . . . ? Pd1 As1 C1 C2 -58.18(18) . . . . ? C6 C1 C2 C3 0.2(3) . . . . ? As1 C1 C2 C3 177.60(17) . . . . ? C1 C2 C3 C4 -0.5(3) . . . . ? C2 C3 C4 C5 0.1(3) . . . . ? C3 C4 C5 C6 0.6(3) . . . . ? C2 C1 C6 C5 0.5(3) . . . . ? As1 C1 C6 C5 -176.86(16) . . . . ? C4 C5 C6 C1 -0.9(3) . . . . ? C13 As1 C7 C8 -101.32(19) . . . . ? C1 As1 C7 C8 7.8(2) . . . . ? Pd1 As1 C7 C8 138.65(17) . . . . ? C13 As1 C7 C12 74.61(18) . . . . ? C1 As1 C7 C12 -176.28(17) . . . . ? Pd1 As1 C7 C12 -45.42(19) . . . . ? C12 C7 C8 C9 -0.5(3) . . . . ? As1 C7 C8 C9 175.35(17) . . . . ? C7 C8 C9 C10 -0.9(4) . . . . ? C8 C9 C10 C11 1.0(4) . . . . ? C9 C10 C11 C12 0.3(4) . . . . ? C10 C11 C12 C7 -1.7(4) . . . . ? C8 C7 C12 C11 1.8(3) . . . . ? As1 C7 C12 C11 -174.19(18) . . . . ? C7 As1 C13 C14 -0.03(19) . . . . ? C1 As1 C13 C14 -110.64(18) . . . . ? Pd1 As1 C13 C14 119.84(16) . . . . ? C7 As1 C13 C18 -176.82(17) . . . . ? C1 As1 C13 C18 72.57(18) . . . . ? Pd1 As1 C13 C18 -56.95(18) . . . . ? C18 C13 C14 C15 0.8(3) . . . . ? As1 C13 C14 C15 -176.00(17) . . . . ? C13 C14 C15 C16 -0.6(3) . . . . ? C14 C15 C16 C17 -0.7(4) . . . . ? C15 C16 C17 C18 1.8(4) . . . . ? C16 C17 C18 C13 -1.7(4) . . . . ? C14 C13 C18 C17 0.4(3) . . . . ? As1 C13 C18 C17 177.24(18) . . . . ? O1A Pd1 O1A N1A 163(100) 2_666 . . . ? O1B Pd1 O1A N1A -5.5(14) . . . . ? O1B Pd1 O1A N1A 174.5(14) 2_666 . . . ? N1 Pd1 O1A N1A 177.5(10) 2_666 . . . ? N1 Pd1 O1A N1A -2.5(10) . . . . ? O1C Pd1 O1A N1A -58(21) 2_666 . . . ? O1C Pd1 O1A N1A 122(21) . . . . ? As1 Pd1 O1A N1A 71.2(17) . . . . ? As1 Pd1 O1A N1A -108.8(17) 2_666 . . . ? N1C Pd1 O1A N1A -1.0(19) . . . . ? N1C Pd1 O1A N1A 179.0(19) 2_666 . . . ? Pd1 O1A N1A O2A -6(3) . . . . ? O1A Pd1 O1B N1B 173.0(10) 2_666 . . . ? O1A Pd1 O1B N1B -7.0(10) . . . . ? O1B Pd1 O1B N1B -68(100) 2_666 . . . ? N1 Pd1 O1B N1B 169.9(6) 2_666 . . . ? N1 Pd1 O1B N1B -10.1(6) . . . . ? O1C Pd1 O1B N1B 170.3(11) 2_666 . . . ? O1C Pd1 O1B N1B -9.7(11) . . . . ? As1 Pd1 O1B N1B -110.9(8) . . . . ? As1 Pd1 O1B N1B 69.1(8) 2_666 . . . ? N1C Pd1 O1B N1B -13(2) . . . . ? N1C Pd1 O1B N1B 167(2) 2_666 . . . ? Pd1 O1B N1B O2B 16.0(15) . . . . ? O1A Pd1 O1C N1C 127(19) 2_666 . . . ? O1A Pd1 O1C N1C -53(19) . . . . ? O1B Pd1 O1C N1C -2.5(14) . . . . ? O1B Pd1 O1C N1C 177.5(14) 2_666 . . . ? N1 Pd1 O1C N1C 177.9(14) 2_666 . . . ? N1 Pd1 O1C N1C -2.1(14) . . . . ? O1C Pd1 O1C N1C 179(100) 2_666 . . . ? As1 Pd1 O1C N1C 76.1(17) . . . . ? As1 Pd1 O1C N1C -103.9(17) 2_666 . . . ? N1C Pd1 O1C N1C 180.000(5) 2_666 . . . ? Pd1 O1C N1C O2C 175(2) . . . . ? O1A Pd1 N1C O1C -176(2) 2_666 . . . ? O1A Pd1 N1C O1C 4(2) . . . . ? O1B Pd1 N1C O1C 175(3) . . . . ? O1B Pd1 N1C O1C -5(3) 2_666 . . . ? N1 Pd1 N1C O1C -166(9) 2_666 . . . ? N1 Pd1 N1C O1C 14(9) . . . . ? O1C Pd1 N1C O1C 180.000(4) 2_666 . . . ? As1 Pd1 N1C O1C -104.7(18) . . . . ? As1 Pd1 N1C O1C 75.3(18) 2_666 . . . ? N1C Pd1 N1C O1C -21(100) 2_666 . . . ? O1A Pd1 N1C O2C 157(9) 2_666 . . . ? O1A Pd1 N1C O2C -23(9) . . . . ? O1B Pd1 N1C O2C 148(11) . . . . ? O1B Pd1 N1C O2C -32(11) 2_666 . . . ? N1 Pd1 N1C O2C 167(4) 2_666 . . . ? N1 Pd1 N1C O2C -13(4) . . . . ? O1C Pd1 N1C O2C 153(9) 2_666 . . . ? O1C Pd1 N1C O2C -27(9) . . . . ? As1 Pd1 N1C O2C -132(10) . . . . ? As1 Pd1 N1C O2C 48(10) 2_666 . . . ? N1C Pd1 N1C O2C -48(100) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 33.65 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.566 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.127 ###END data_4 _database_code_depnum_ccdc_archive 'CCDC 866985' #TrackingRef '- all_1_4_cif.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis-(Triphenylphosphine)dinitro-platinum(II) ; _chemical_formula_moiety 'C38 H34 Cl4 N2 O4 P2 Pt' _chemical_formula_sum 'C38 H34 Cl4 N2 O4 P2 Pt' _chemical_formula_weight 981.50 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.471(5) _cell_length_b 7.953(5) _cell_length_c 23.261(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3787(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 553 _cell_measurement_theta_min 3.2556 _cell_measurement_theta_max 32.5058 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 4.115 _exptl_absorpt_correction_T_min 0.97391 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Atlas (Gemini ultra Mo) ; _diffrn_detector_area_resol_mean 10.3795 _diffrn_reflns_number 2820 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.2057 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 32.92 _reflns_number_total 6847 _reflns_number_gt 3326 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1997)' _computing_publication_material 'ENCIFER v1.4' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6847 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_ref 0.0338 _refine_ls_wR_factor_gt 0.0298 _refine_ls_goodness_of_fit_ref 0.765 _refine_ls_restrained_S_all 0.765 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pt1 Pt 0.5000 0.0000 0.5000 0.01341(2) Uani 1 2 d S . . Cl1 Cl 0.23152(3) 0.24708(9) 0.17150(3) 0.05341(18) Uani 1 1 d . . . Cl2 Cl 0.35151(3) 0.36565(8) 0.22591(3) 0.04412(15) Uani 1 1 d . . . P1 P 0.56393(2) -0.14737(6) 0.56595(2) 0.01481(9) Uani 1 1 d . . . 01 O 0.37835(7) -0.04712(17) 0.55651(6) 0.0304(4) Uani 1 1 d . . . 02 O 0.43972(7) 0.13385(18) 0.59875(6) 0.0288(3) Uani 1 1 d . . . N1 N 0.42955(8) 0.03158(18) 0.55940(7) 0.0196(4) Uani 1 1 d . . . C1 C 0.52158(9) -0.2718(2) 0.62035(8) 0.0171(4) Uani 1 1 d . . . C2 C 0.48497(9) -0.1922(2) 0.66265(8) 0.0241(5) Uani 1 1 d . . . H2 H 0.4821 -0.0730 0.6630 0.029 Uiso 1 1 calc R . . C3 C 0.45281(11) -0.2840(3) 0.70417(9) 0.0297(5) Uani 1 1 d . . . H3 H 0.4274 -0.2281 0.7325 0.036 Uiso 1 1 calc R . . C4 C 0.45744(11) -0.4578(3) 0.70467(9) 0.0318(6) Uani 1 1 d . . . H4 H 0.4355 -0.5211 0.7334 0.038 Uiso 1 1 calc R . . C5 C 0.49403(12) -0.5385(2) 0.66335(9) 0.0311(5) Uani 1 1 d . . . H5 H 0.4974 -0.6576 0.6637 0.037 Uiso 1 1 calc R . . C6 C 0.52600(10) -0.4466(2) 0.62121(9) 0.0228(4) Uani 1 1 d . . . H6 H 0.5510 -0.5031 0.5928 0.027 Uiso 1 1 calc R . . C7 C 0.61430(8) -0.0041(3) 0.60718(7) 0.0165(3) Uani 1 1 d . . . C8 C 0.62447(9) 0.1594(2) 0.58842(8) 0.0222(4) Uani 1 1 d . . . H8 H 0.6052 0.1964 0.5535 0.027 Uiso 1 1 calc R . . C9 C 0.66263(10) 0.2692(3) 0.62033(9) 0.0258(5) Uani 1 1 d . . . H9 H 0.6698 0.3807 0.6071 0.031 Uiso 1 1 calc R . . C10 C 0.69008(10) 0.2167(3) 0.67105(10) 0.0272(5) Uani 1 1 d . . . H10 H 0.7153 0.2928 0.6933 0.033 Uiso 1 1 calc R . . C11 C 0.68118(10) 0.0537(3) 0.68997(9) 0.0255(5) Uani 1 1 d . . . H11 H 0.7013 0.0174 0.7246 0.031 Uiso 1 1 calc R . . C12 C 0.64311(10) -0.0569(2) 0.65873(8) 0.0229(4) Uani 1 1 d . . . H12 H 0.6365 -0.1684 0.6722 0.027 Uiso 1 1 calc R . . C13 C 0.61789(9) -0.2928(2) 0.52916(8) 0.0163(4) Uani 1 1 d . . . C14 C 0.59034(10) -0.4039(2) 0.48938(8) 0.0209(5) Uani 1 1 d . . . H14 H 0.5446 -0.4018 0.4827 0.025 Uiso 1 1 calc R . . C15 C 0.62902(10) -0.5170(3) 0.45957(8) 0.0256(4) Uani 1 1 d . . . H15 H 0.6098 -0.5937 0.4332 0.031 Uiso 1 1 calc R . . C16 C 0.69557(10) -0.5175(3) 0.46843(9) 0.0285(5) Uani 1 1 d . . . H16 H 0.7224 -0.5942 0.4479 0.034 Uiso 1 1 calc R . . C17 C 0.72358(10) -0.4067(2) 0.50713(10) 0.0277(5) Uani 1 1 d . . . H17 H 0.7696 -0.4068 0.5126 0.033 Uiso 1 1 calc R . . C18 C 0.68506(9) -0.2962(2) 0.53788(9) 0.0216(4) Uani 1 1 d . . . H18 H 0.7045 -0.2224 0.5650 0.026 Uiso 1 1 calc R . . C19 C 0.31448(12) 0.2974(3) 0.16158(10) 0.0430(7) Uani 1 1 d . . . H19A H 0.3182 0.3871 0.1323 0.052 Uiso 1 1 calc R . . H19B H 0.3379 0.1972 0.1470 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01205(3) 0.01456(3) 0.01363(3) -0.00007(5) 0.00040(6) 0.00111(6) Cl1 0.0484(4) 0.0645(4) 0.0474(4) -0.0041(4) 0.0195(3) -0.0223(4) Cl2 0.0541(4) 0.0450(3) 0.0333(3) 0.0086(3) -0.0024(3) 0.0041(3) P1 0.0134(2) 0.0149(2) 0.0161(2) 0.0007(2) -0.0007(2) 0.0007(2) 01 0.0203(8) 0.0354(9) 0.0355(9) 0.0004(7) 0.0073(7) -0.0039(6) 02 0.0337(9) 0.0296(8) 0.0230(8) -0.0060(7) 0.0038(7) 0.0034(7) N1 0.0217(9) 0.0204(10) 0.0168(8) 0.0026(6) 0.0027(7) 0.0064(7) C1 0.0141(9) 0.0204(9) 0.0167(9) 0.0035(8) -0.0040(7) -0.0034(8) C2 0.0262(13) 0.0241(10) 0.0221(10) 0.0027(8) 0.0038(8) 0.0034(8) C3 0.0292(12) 0.0373(13) 0.0225(11) 0.0044(9) 0.0070(9) -0.0003(11) C4 0.0307(12) 0.0388(14) 0.0258(11) 0.0095(9) 0.0011(10) -0.0134(10) C5 0.0416(14) 0.0220(11) 0.0297(10) 0.0031(7) -0.0004(12) -0.0116(11) C6 0.0274(11) 0.0207(9) 0.0203(10) 0.0008(8) -0.0004(9) -0.0043(8) C7 0.0138(8) 0.0175(8) 0.0181(8) -0.0030(10) 0.0006(6) 0.0015(11) C8 0.0223(11) 0.0219(10) 0.0224(10) 0.0021(8) -0.0012(8) -0.0007(9) C9 0.0263(12) 0.0197(10) 0.0313(12) -0.0015(9) -0.0009(10) -0.0054(9) C10 0.0203(12) 0.0298(12) 0.0316(12) -0.0114(10) -0.0007(10) -0.0035(10) C11 0.0241(12) 0.0324(11) 0.0200(10) -0.0027(8) -0.0056(9) 0.0005(9) C12 0.0224(11) 0.0212(9) 0.0250(11) 0.0014(8) -0.0037(9) 0.0006(8) C13 0.0168(10) 0.0145(9) 0.0175(10) 0.0034(7) 0.0014(8) 0.0012(8) C14 0.0191(10) 0.0195(9) 0.0241(13) -0.0003(7) -0.0017(8) 0.0000(8) C15 0.0315(11) 0.0215(11) 0.0240(10) -0.0016(9) 0.0000(8) 0.0018(10) C16 0.0317(11) 0.0252(12) 0.0286(11) 0.0005(10) 0.0093(9) 0.0132(11) C17 0.0185(10) 0.0270(10) 0.0377(14) 0.0018(10) 0.0002(10) 0.0062(8) C18 0.0191(11) 0.0199(10) 0.0259(11) 0.0020(8) -0.0007(9) 0.0007(8) C19 0.0409(16) 0.0541(18) 0.0339(14) -0.0016(12) 0.0120(12) -0.0072(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.0130(16) . ? Pt1 N1 2.0130(16) 5_656 ? Pt1 P1 2.3323(7) 5_656 ? Pt1 P1 2.3323(7) . ? Cl1 C19 1.760(2) . ? Cl2 C19 1.763(2) . ? P1 C7 1.811(2) . ? P1 C13 1.8140(19) . ? P1 C1 1.8252(19) . ? 01 N1 1.223(2) . ? 02 N1 1.2420(19) . ? C1 C2 1.389(3) . ? C1 C6 1.394(3) . ? C2 C3 1.378(3) . ? C2 H2 0.9500 . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.377(3) . ? C4 H4 0.9500 . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.388(3) . ? C7 C12 1.401(2) . ? C8 C9 1.387(3) . ? C8 H8 0.9500 . ? C9 C10 1.372(3) . ? C9 H9 0.9500 . ? C10 C11 1.381(3) . ? C10 H10 0.9500 . ? C11 C12 1.381(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.390(3) . ? C13 C14 1.398(3) . ? C14 C15 1.384(3) . ? C14 H14 0.9500 . ? C15 C16 1.378(3) . ? C15 H15 0.9500 . ? C16 C17 1.384(3) . ? C16 H16 0.9500 . ? C17 C18 1.380(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N1 180.00(6) . 5_656 ? N1 Pt1 P1 89.24(5) . 5_656 ? N1 Pt1 P1 90.76(5) 5_656 5_656 ? N1 Pt1 P1 90.76(5) . . ? N1 Pt1 P1 89.24(5) 5_656 . ? P1 Pt1 P1 180.000(18) 5_656 . ? C7 P1 C13 107.71(9) . . ? C7 P1 C1 104.13(9) . . ? C13 P1 C1 105.71(9) . . ? C7 P1 Pt1 110.59(7) . . ? C13 P1 Pt1 110.59(7) . . ? C1 P1 Pt1 117.51(6) . . ? 01 N1 02 121.30(17) . . ? 01 N1 Pt1 120.83(13) . . ? 02 N1 Pt1 117.87(13) . . ? C2 C1 C6 118.64(18) . . ? C2 C1 P1 120.02(15) . . ? C6 C1 P1 121.32(16) . . ? C3 C2 C1 120.83(19) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 120.1(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.7(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.31(19) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.3(2) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 119.12(18) . . ? C8 C7 P1 120.56(14) . . ? C12 C7 P1 120.31(16) . . ? C9 C8 C7 120.43(18) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 119.9(2) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.4(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 120.3(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 119.83(19) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C18 C13 C14 118.89(18) . . ? C18 C13 P1 123.08(15) . . ? C14 C13 P1 118.01(14) . . ? C15 C14 C13 120.75(19) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 119.5(2) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 120.35(19) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 120.37(19) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C13 120.12(19) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? Cl1 C19 Cl2 111.94(13) . . ? Cl1 C19 H19A 109.2 . . ? Cl2 C19 H19A 109.2 . . ? Cl1 C19 H19B 109.2 . . ? Cl2 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 P1 C7 -87.63(8) . . . . ? N1 Pt1 P1 C7 92.37(8) 5_656 . . . ? P1 Pt1 P1 C7 -25(100) 5_656 . . . ? N1 Pt1 P1 C13 153.14(8) . . . . ? N1 Pt1 P1 C13 -26.86(8) 5_656 . . . ? P1 Pt1 P1 C13 -145(100) 5_656 . . . ? N1 Pt1 P1 C1 31.69(8) . . . . ? N1 Pt1 P1 C1 -148.31(8) 5_656 . . . ? P1 Pt1 P1 C1 94(100) 5_656 . . . ? N1 Pt1 N1 01 -160.7(3) 5_656 . . . ? P1 Pt1 N1 01 72.85(14) 5_656 . . . ? P1 Pt1 N1 01 -107.15(14) . . . . ? N1 Pt1 N1 02 19.63(12) 5_656 . . . ? P1 Pt1 N1 02 -106.83(13) 5_656 . . . ? P1 Pt1 N1 02 73.17(13) . . . . ? C7 P1 C1 C2 55.42(17) . . . . ? C13 P1 C1 C2 168.79(15) . . . . ? Pt1 P1 C1 C2 -67.26(16) . . . . ? C7 P1 C1 C6 -123.40(17) . . . . ? C13 P1 C1 C6 -10.03(19) . . . . ? Pt1 P1 C1 C6 113.92(16) . . . . ? C6 C1 C2 C3 -1.0(3) . . . . ? P1 C1 C2 C3 -179.82(16) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C3 C4 C5 C6 -0.2(4) . . . . ? C4 C5 C6 C1 0.2(3) . . . . ? C2 C1 C6 C5 0.4(3) . . . . ? P1 C1 C6 C5 179.24(16) . . . . ? C13 P1 C7 C8 104.35(16) . . . . ? C1 P1 C7 C8 -143.72(15) . . . . ? Pt1 P1 C7 C8 -16.61(16) . . . . ? C13 P1 C7 C12 -76.15(16) . . . . ? C1 P1 C7 C12 35.79(17) . . . . ? Pt1 P1 C7 C12 162.90(13) . . . . ? C12 C7 C8 C9 0.0(3) . . . . ? P1 C7 C8 C9 179.47(15) . . . . ? C7 C8 C9 C10 -0.6(3) . . . . ? C8 C9 C10 C11 1.5(3) . . . . ? C9 C10 C11 C12 -1.7(3) . . . . ? C10 C11 C12 C7 1.1(3) . . . . ? C8 C7 C12 C11 -0.2(3) . . . . ? P1 C7 C12 C11 -179.70(16) . . . . ? C7 P1 C13 C18 5.75(19) . . . . ? C1 P1 C13 C18 -105.12(17) . . . . ? Pt1 P1 C13 C18 126.70(15) . . . . ? C7 P1 C13 C14 -172.93(14) . . . . ? C1 P1 C13 C14 76.21(16) . . . . ? Pt1 P1 C13 C14 -51.97(16) . . . . ? C18 C13 C14 C15 0.7(3) . . . . ? P1 C13 C14 C15 179.47(15) . . . . ? C13 C14 C15 C16 -1.3(3) . . . . ? C14 C15 C16 C17 0.5(3) . . . . ? C15 C16 C17 C18 0.9(3) . . . . ? C16 C17 C18 C13 -1.5(3) . . . . ? C14 C13 C18 C17 0.7(3) . . . . ? P1 C13 C18 C17 -178.00(15) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 32.92 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.610 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.085