Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Mak, Thomas C. W.' 'Song, Hai-Bin' 'Zhang, Zheng-Zhi' _publ_contact_author_name 'Prof Thomas C W Mak' _publ_contact_author_address ; The Chinese University of Hong Kong Department of Chemistry Shatin New Territories Hong Kong SAR, P R CHINA ; _publ_contact_author_email 'TCWMAK@CUHK.EDU.HK' _publ_section_title ; Synthesis and Structure Study of Late Transition Metal Complexes of N-[(Diphenylphosphino)methyl]-2-pyridinamine and N,N'-Cyclohexyl-[(diphenylphosphino)methyl]-2-pyridinamine ; data_compd1 #compound1 _database_code_CSD 171811 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H18 Cl N2 O5 P' _chemical_formula_weight 408.76 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3745(15) _cell_length_b 9.4683(9) _cell_length_c 16.8207(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.295(10) _cell_angle_gamma 90.00 _cell_volume 1954.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.309 _exptl_absorpt_correction_type PSI-Scan _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4952 _diffrn_reflns_av_R_equivalents 0.0156 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3844 _reflns_number_gt 2706 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0405P)^2^+1.1089P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3844 _refine_ls_number_parameters 272 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1195 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.286 _refine_ls_shift/su_max 0.098 _refine_ls_shift/su_mean 0.008 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 P1 P 0.13425(6) 0.66428(9) 0.04013(5) 0.0411(2) Uani 1 1 d . . . O1 O 0.04769(16) 0.6070(3) 0.08498(13) 0.0530(6) Uani 1 1 d . . . N1 N 0.1762(2) 0.4251(3) -0.03997(16) 0.0483(7) Uani 1 1 d . . . H1A H 0.1071 0.4321 -0.0541 0.058 Uiso 1 1 calc R . . N2 N 0.3361(2) 0.3004(3) -0.04757(16) 0.0467(7) Uani 1 1 d . . . H2B H 0.3693 0.3573 -0.0129 0.056 Uiso 1 1 calc R . . C1 C 0.0810(2) 0.7473(3) -0.05229(19) 0.0429(7) Uani 1 1 d . . . C2 C 0.1281(3) 0.7363(4) -0.1225(2) 0.0588(9) Uani 1 1 d . . . H2A H 0.1923 0.6855 -0.1230 0.071 Uiso 1 1 calc R . . C3 C 0.0798(4) 0.8011(4) -0.1918(2) 0.0703(11) Uani 1 1 d . . . H3A H 0.1116 0.7931 -0.2389 0.084 Uiso 1 1 calc R . . C4 C -0.0140(3) 0.8764(4) -0.1916(3) 0.0713(11) Uani 1 1 d . . . H4A H -0.0461 0.9194 -0.2384 0.086 Uiso 1 1 calc R . . C5 C -0.0607(3) 0.8887(4) -0.1227(3) 0.0708(11) Uani 1 1 d . . . H5A H -0.1245 0.9405 -0.1226 0.085 Uiso 1 1 calc R . . C6 C -0.0139(3) 0.8251(4) -0.0535(2) 0.0566(9) Uani 1 1 d . . . H6A H -0.0463 0.8344 -0.0068 0.068 Uiso 1 1 calc R . . C7 C 0.2222(2) 0.7872(3) 0.09857(19) 0.0422(7) Uani 1 1 d . . . C8 C 0.2225(3) 0.7900(4) 0.1809(2) 0.0608(10) Uani 1 1 d . . . H8A H 0.1765 0.7305 0.2050 0.073 Uiso 1 1 calc R . . C9 C 0.2912(4) 0.8814(5) 0.2272(2) 0.0748(12) Uani 1 1 d . . . H9A H 0.2922 0.8819 0.2826 0.090 Uiso 1 1 calc R . . C10 C 0.3576(3) 0.9708(4) 0.1923(3) 0.0717(12) Uani 1 1 d . . . H10A H 0.4036 1.0319 0.2239 0.086 Uiso 1 1 calc R . . C11 C 0.3567(3) 0.9711(4) 0.1107(3) 0.0681(11) Uani 1 1 d . . . H11A H 0.4015 1.0329 0.0870 0.082 Uiso 1 1 calc R . . C12 C 0.2893(3) 0.8797(4) 0.0639(2) 0.0561(9) Uani 1 1 d . . . H12A H 0.2887 0.8801 0.0086 0.067 Uiso 1 1 calc R . . C13 C 0.2282(2) 0.5290(3) 0.0156(2) 0.0457(8) Uani 1 1 d . . . H13A H 0.2875 0.5732 -0.0079 0.055 Uiso 1 1 calc R . . H13B H 0.2591 0.4817 0.0644 0.055 Uiso 1 1 calc R . . C14 C 0.2288(2) 0.3198(3) -0.07035(18) 0.0397(7) Uani 1 1 d . . . C15 C 0.1768(3) 0.2251(4) -0.1268(2) 0.0507(8) Uani 1 1 d . . . H15A H 0.1029 0.2350 -0.1445 0.061 Uiso 1 1 calc R . . C16 C 0.2344(3) 0.1195(4) -0.1553(2) 0.0607(10) Uani 1 1 d . . . H16A H 0.1994 0.0572 -0.1929 0.073 Uiso 1 1 calc R . . C17 C 0.3453(3) 0.1023(4) -0.1295(2) 0.0604(10) Uani 1 1 d . . . H17A H 0.3842 0.0281 -0.1485 0.072 Uiso 1 1 calc R . . C18 C 0.3942(3) 0.1952(4) -0.0768(2) 0.0570(9) Uani 1 1 d . . . H18A H 0.4685 0.1876 -0.0601 0.068 Uiso 1 1 calc R . . Cl1 Cl 0.53948(7) 0.35315(11) 0.13173(6) 0.0621(3) Uani 1 1 d D . . O2 O 0.6258(2) 0.4440(3) 0.15877(17) 0.0860(9) Uani 1 1 d D . . O3 O 0.5666(7) 0.2595(8) 0.0744(4) 0.103(3) Uani 0.70 1 d PDU . . O4 O 0.5255(6) 0.2703(8) 0.2012(3) 0.145(3) Uani 0.70 1 d PD . . O5 O 0.4432(5) 0.4199(11) 0.1072(5) 0.181(5) Uani 0.70 1 d PD . . O3' O 0.5719(18) 0.2331(16) 0.0947(14) 0.141(11) Uani 0.30 1 d PDU . . O4' O 0.4436(9) 0.3554(19) 0.1627(12) 0.128(7) Uani 0.30 1 d PD . . O5' O 0.4998(9) 0.4329(11) 0.0611(6) 0.103(5) Uani 0.30 1 d PD . . 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 P1 0.0314(4) 0.0378(4) 0.0537(5) -0.0023(4) 0.0039(3) 0.0021(3) O1 0.0385(11) 0.0575(15) 0.0637(15) 0.0027(12) 0.0092(10) -0.0048(11) N1 0.0314(13) 0.0395(15) 0.0720(18) -0.0101(14) -0.0014(12) 0.0022(12) N2 0.0407(14) 0.0399(15) 0.0574(16) -0.0079(13) -0.0025(12) 0.0042(12) C1 0.0384(16) 0.0368(17) 0.0524(19) -0.0041(14) 0.0021(14) 0.0021(14) C2 0.058(2) 0.058(2) 0.060(2) -0.0013(18) 0.0111(18) 0.0140(18) C3 0.089(3) 0.068(3) 0.055(2) 0.000(2) 0.012(2) 0.004(2) C4 0.073(3) 0.062(3) 0.073(3) 0.013(2) -0.016(2) 0.001(2) C5 0.057(2) 0.066(3) 0.088(3) 0.014(2) 0.003(2) 0.021(2) C6 0.0506(19) 0.052(2) 0.068(2) 0.0032(18) 0.0102(17) 0.0136(17) C7 0.0354(15) 0.0358(16) 0.0549(19) -0.0051(14) 0.0035(14) 0.0063(13) C8 0.074(2) 0.050(2) 0.056(2) 0.0063(17) -0.0004(19) -0.0007(19) C9 0.095(3) 0.068(3) 0.055(2) -0.011(2) -0.015(2) 0.008(3) C10 0.054(2) 0.054(2) 0.102(3) -0.032(2) -0.009(2) 0.004(2) C11 0.048(2) 0.060(2) 0.099(3) -0.026(2) 0.021(2) -0.0105(18) C12 0.0459(18) 0.057(2) 0.068(2) -0.0155(18) 0.0180(17) -0.0046(17) C13 0.0351(15) 0.0365(17) 0.063(2) -0.0048(15) -0.0012(14) 0.0031(14) C14 0.0359(15) 0.0368(17) 0.0462(17) 0.0048(14) 0.0041(13) -0.0016(13) C15 0.0417(17) 0.053(2) 0.055(2) -0.0057(17) -0.0013(15) -0.0069(16) C16 0.070(2) 0.057(2) 0.055(2) -0.0163(18) 0.0034(18) -0.0090(19) C17 0.066(2) 0.053(2) 0.061(2) -0.0131(18) 0.0066(18) 0.0134(19) C18 0.0488(19) 0.058(2) 0.063(2) -0.0078(18) 0.0020(17) 0.0165(17) Cl1 0.0492(5) 0.0765(7) 0.0600(6) -0.0168(5) 0.0042(4) -0.0011(5) O2 0.087(2) 0.087(2) 0.0799(19) -0.0051(17) -0.0062(16) -0.0229(18) O3 0.090(5) 0.128(7) 0.090(4) -0.066(5) 0.008(3) 0.006(5) O4 0.175(6) 0.182(7) 0.074(3) 0.024(4) 0.005(4) -0.108(6) O5 0.085(5) 0.245(12) 0.192(9) -0.125(8) -0.068(5) 0.104(7) O3' 0.115(15) 0.032(6) 0.28(3) 0.001(10) 0.055(15) 0.036(8) O4' 0.086(11) 0.159(16) 0.155(17) -0.001(13) 0.080(12) -0.025(11) O5' 0.049(6) 0.079(8) 0.164(12) -0.011(8) -0.049(7) -0.021(6) _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 P1 O1 1.488(2) . ? P1 C1 1.791(3) . ? P1 C7 1.798(3) . ? P1 C13 1.813(3) . ? N1 C14 1.328(4) . ? N1 C13 1.450(4) . ? N2 C14 1.347(4) . ? N2 C18 1.357(4) . ? C1 C2 1.386(4) . ? C1 C6 1.384(4) . ? C2 C3 1.385(5) . ? C3 C4 1.363(5) . ? C4 C5 1.365(5) . ? C5 C6 1.372(5) . ? C7 C8 1.385(5) . ? C7 C12 1.385(5) . ? C8 C9 1.383(5) . ? C9 C10 1.363(6) . ? C10 C11 1.372(6) . ? C11 C12 1.378(5) . ? C14 C15 1.402(4) . ? C15 C16 1.351(5) . ? C16 C17 1.396(5) . ? C17 C18 1.338(5) . ? Cl1 O5 1.366(4) . ? Cl1 O4' 1.354(5) . ? Cl1 O3' 1.380(6) . ? Cl1 O3 1.383(4) . ? Cl1 O2 1.402(3) . ? Cl1 O4 1.436(4) . ? Cl1 O5' 1.440(5) . ? O4 O4' 1.389(17) . ? O5 O5' 1.115(12) . ? O5 O4' 1.115(17) . ? 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 O1 P1 C1 112.97(13) . . ? O1 P1 C7 112.54(14) . . ? C1 P1 C7 108.73(15) . . ? O1 P1 C13 112.45(15) . . ? C1 P1 C13 106.75(15) . . ? C7 P1 C13 102.75(13) . . ? C14 N1 C13 123.9(2) . . ? C14 N2 C18 123.1(3) . . ? C2 C1 C6 118.4(3) . . ? C2 C1 P1 123.9(2) . . ? C6 C1 P1 117.6(3) . . ? C1 C2 C3 120.1(3) . . ? C4 C3 C2 120.4(4) . . ? C5 C4 C3 120.0(4) . . ? C4 C5 C6 120.3(4) . . ? C5 C6 C1 120.8(3) . . ? C8 C7 C12 118.9(3) . . ? C8 C7 P1 118.9(3) . . ? C12 C7 P1 122.2(3) . . ? C9 C8 C7 119.9(4) . . ? C10 C9 C8 120.5(4) . . ? C9 C10 C11 120.3(4) . . ? C10 C11 C12 119.8(4) . . ? C11 C12 C7 120.6(4) . . ? N1 C13 P1 112.4(2) . . ? N1 C14 N2 120.5(3) . . ? N1 C14 C15 122.4(3) . . ? N2 C14 C15 117.2(3) . . ? C16 C15 C14 119.8(3) . . ? C15 C16 C17 121.2(3) . . ? C18 C17 C16 118.2(3) . . ? C17 C18 N2 120.5(3) . . ? O5 Cl1 O4' 48.4(8) . . ? O5 Cl1 O3' 122.5(10) . . ? O4' Cl1 O3' 120.4(13) . . ? O5 Cl1 O3 111.4(4) . . ? O4' Cl1 O3 125.5(8) . . ? O3' Cl1 O3 17.6(14) . . ? O5 Cl1 O2 114.4(5) . . ? O4' Cl1 O2 122.3(8) . . ? O3' Cl1 O2 113.5(10) . . ? O3 Cl1 O2 112.2(4) . . ? O5 Cl1 O4 108.0(5) . . ? O4' Cl1 O4 59.6(8) . . ? O3' Cl1 O4 89.4(12) . . ? O3 Cl1 O4 106.4(5) . . ? O2 Cl1 O4 103.7(2) . . ? O5 Cl1 O5' 46.7(5) . . ? O4' Cl1 O5' 94.9(10) . . ? O3' Cl1 O5' 98.5(12) . . ? O3 Cl1 O5' 81.3(7) . . ? O2 Cl1 O5' 96.4(4) . . ? O4 Cl1 O5' 153.4(5) . . ? O4' O4 Cl1 57.3(4) . . ? O5' O5 O4' 134.8(8) . . ? O5' O5 Cl1 70.1(4) . . ? O4' O5 Cl1 65.3(5) . . ? O4 O4' O5 129.4(6) . . ? O4 O4' Cl1 63.1(5) . . ? O5 O4' Cl1 66.4(5) . . ? O5 O5' Cl1 63.1(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.492 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.044 #============================================END data_compd2 #compound2 _database_code_CSD 171812 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H34 Fe N4 O3 P2' _chemical_formula_weight 724.49 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.007(5) _cell_length_b 8.964(2) _cell_length_c 19.136(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.400(5) _cell_angle_gamma 90.00 _cell_volume 3519.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.630766 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11336 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.03 _reflns_number_total 4220 _reflns_number_gt 2786 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0526P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4220 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 0.24290(4) 0.2500 0.02860(12) Uani 1 2 d S . . P1 P -0.06810(2) 0.24170(6) 0.14543(2) 0.02876(13) Uani 1 1 d . . . N1 N -0.01485(8) 0.0049(2) 0.08829(9) 0.0415(4) Uani 1 1 d . . . H1A H -0.0442 -0.0614 0.0893 0.050 Uiso 1 1 calc R . . N2 N 0.09340(9) 0.0599(2) 0.09179(9) 0.0460(5) Uani 1 1 d . . . C1 C 0.0000 0.0442(3) 0.2500 0.0351(6) Uani 1 2 d S . . O1 O 0.0000 -0.0842(2) 0.2500 0.0571(6) Uani 1 2 d S . . C2 C 0.05463(11) 0.3422(3) 0.20880(11) 0.0445(5) Uani 1 1 d . . . O2 O 0.08962(9) 0.4061(2) 0.18029(9) 0.0783(6) Uani 1 1 d . . . C11 C -0.09558(9) 0.4252(2) 0.10821(11) 0.0373(5) Uani 1 1 d . . . C12 C -0.07697(11) 0.4847(3) 0.04910(14) 0.0531(6) Uani 1 1 d . . . H12A H -0.0504 0.4301 0.0255 0.064 Uiso 1 1 calc R . . C13 C -0.09800(12) 0.6267(3) 0.02491(17) 0.0704(8) Uani 1 1 d . . . H13A H -0.0852 0.6665 -0.0148 0.084 Uiso 1 1 calc R . . C14 C -0.13682(15) 0.7069(3) 0.0585(2) 0.0759(10) Uani 1 1 d . . . H14A H -0.1504 0.8018 0.0420 0.091 Uiso 1 1 calc R . . C15 C -0.15635(16) 0.6488(3) 0.11700(17) 0.0805(9) Uani 1 1 d . . . H15A H -0.1831 0.7042 0.1401 0.097 Uiso 1 1 calc R . . C16 C -0.13599(13) 0.5071(3) 0.14149(14) 0.0627(7) Uani 1 1 d . . . H16A H -0.1497 0.4672 0.1806 0.075 Uiso 1 1 calc R . . C21 C -0.14554(9) 0.1415(2) 0.13750(10) 0.0320(4) Uani 1 1 d . . . C22 C -0.18749(10) 0.1288(2) 0.07066(11) 0.0412(5) Uani 1 1 d . . . H22A H -0.1768 0.1740 0.0310 0.049 Uiso 1 1 calc R . . C23 C -0.24499(11) 0.0492(3) 0.06302(13) 0.0496(6) Uani 1 1 d . . . H23A H -0.2727 0.0409 0.0182 0.060 Uiso 1 1 calc R . . C24 C -0.26117(10) -0.0173(3) 0.12134(13) 0.0509(6) Uani 1 1 d . . . H24A H -0.2996 -0.0718 0.1160 0.061 Uiso 1 1 calc R . . C25 C -0.22111(11) -0.0037(3) 0.18705(13) 0.0514(6) Uani 1 1 d . . . H25A H -0.2327 -0.0476 0.2266 0.062 Uiso 1 1 calc R . . C26 C -0.16298(10) 0.0753(3) 0.19560(11) 0.0422(5) Uani 1 1 d . . . H26A H -0.1358 0.0834 0.2407 0.051 Uiso 1 1 calc R . . C31 C -0.03535(10) 0.1562(2) 0.07251(10) 0.0386(5) Uani 1 1 d . . . H31A H -0.0686 0.1584 0.0287 0.046 Uiso 1 1 calc R . . H31B H 0.0014 0.2146 0.0648 0.046 Uiso 1 1 calc R . . C32 C 0.04902(10) -0.0395(2) 0.10189(10) 0.0392(5) Uani 1 1 d . . . C33 C 0.06549(13) -0.1857(3) 0.12451(13) 0.0517(6) Uani 1 1 d . . . H33A H 0.0336 -0.2528 0.1313 0.062 Uiso 1 1 calc R . . C34 C 0.12875(15) -0.2274(3) 0.13631(15) 0.0639(7) Uani 1 1 d . . . H34A H 0.1407 -0.3237 0.1518 0.077 Uiso 1 1 calc R . . C35 C 0.17558(13) -0.1276(3) 0.12549(14) 0.0628(7) Uani 1 1 d . . . H35A H 0.2192 -0.1553 0.1326 0.075 Uiso 1 1 calc R . . C36 C 0.15580(12) 0.0126(3) 0.10411(13) 0.0566(6) Uani 1 1 d . . . H36A H 0.1874 0.0806 0.0975 0.068 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 Fe1 0.0281(2) 0.0321(2) 0.02502(19) 0.000 0.00457(14) 0.000 P1 0.0280(2) 0.0321(3) 0.0258(2) 0.0008(2) 0.00507(19) 0.0031(2) N1 0.0384(10) 0.0411(10) 0.0462(10) -0.0063(9) 0.0119(8) 0.0004(8) N2 0.0431(10) 0.0497(11) 0.0465(10) -0.0017(9) 0.0124(8) 0.0056(9) C1 0.0395(16) 0.0424(18) 0.0235(13) 0.000 0.0072(11) 0.000 O1 0.0948(18) 0.0350(13) 0.0462(13) 0.000 0.0255(12) 0.000 C2 0.0436(12) 0.0526(14) 0.0355(11) 0.0030(11) 0.0043(9) -0.0095(11) O2 0.0806(13) 0.0953(16) 0.0637(11) 0.0102(11) 0.0262(10) -0.0405(12) C11 0.0347(11) 0.0328(11) 0.0402(11) 0.0039(9) -0.0010(8) 0.0022(9) C12 0.0378(12) 0.0526(14) 0.0688(16) 0.0222(13) 0.0115(11) 0.0011(11) C13 0.0493(15) 0.0588(17) 0.096(2) 0.0408(17) -0.0010(14) -0.0096(14) C14 0.0685(19) 0.0352(14) 0.107(3) 0.0166(16) -0.0181(18) 0.0013(14) C15 0.095(2) 0.0552(17) 0.083(2) -0.0076(17) -0.0001(18) 0.0361(17) C16 0.0815(19) 0.0509(15) 0.0539(15) -0.0002(13) 0.0110(14) 0.0272(14) C21 0.0286(10) 0.0312(10) 0.0353(10) -0.0020(9) 0.0046(8) 0.0032(8) C22 0.0394(12) 0.0449(13) 0.0369(11) -0.0012(10) 0.0031(9) 0.0007(10) C23 0.0370(12) 0.0511(14) 0.0544(14) -0.0081(12) -0.0043(10) -0.0010(11) C24 0.0342(12) 0.0451(13) 0.0721(16) -0.0051(13) 0.0085(11) -0.0034(10) C25 0.0436(13) 0.0583(15) 0.0556(14) 0.0061(12) 0.0176(11) -0.0061(12) C26 0.0345(11) 0.0537(14) 0.0380(11) 0.0000(10) 0.0071(9) -0.0014(10) C31 0.0397(11) 0.0474(13) 0.0296(10) 0.0009(10) 0.0095(8) 0.0079(10) C32 0.0453(12) 0.0436(12) 0.0309(10) -0.0062(9) 0.0129(9) 0.0077(10) C33 0.0644(16) 0.0417(13) 0.0533(14) -0.0016(12) 0.0221(12) 0.0099(12) C34 0.0755(19) 0.0565(17) 0.0631(16) 0.0054(13) 0.0225(14) 0.0274(15) C35 0.0506(15) 0.079(2) 0.0592(15) -0.0070(15) 0.0123(12) 0.0279(15) C36 0.0447(14) 0.0705(18) 0.0576(15) -0.0062(14) 0.0178(11) 0.0031(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 Fe1 C2 1.766(2) 2 ? Fe1 C2 1.766(2) . ? Fe1 C1 1.781(3) . ? Fe1 P1 2.1958(6) 2 ? Fe1 P1 2.1958(6) . ? P1 C11 1.835(2) . ? P1 C21 1.836(2) . ? P1 C31 1.849(2) . ? N1 C32 1.370(3) . ? N1 C31 1.435(3) . ? N2 C32 1.333(3) . ? N2 C36 1.349(3) . ? C1 O1 1.151(3) . ? C2 O2 1.157(3) . ? C11 C16 1.377(3) . ? C11 C12 1.381(3) . ? C12 C13 1.393(3) . ? C13 C14 1.349(4) . ? C14 C15 1.375(4) . ? C15 C16 1.390(4) . ? C21 C26 1.378(3) . ? C21 C22 1.393(3) . ? C22 C23 1.383(3) . ? C23 C24 1.371(3) . ? C24 C25 1.360(3) . ? C25 C26 1.391(3) . ? C32 C33 1.400(3) . ? C33 C34 1.352(4) . ? C34 C35 1.377(4) . ? C35 C36 1.359(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C2 119.49(16) 2 . ? C2 Fe1 C1 120.26(8) 2 . ? C2 Fe1 C1 120.26(8) . . ? C2 Fe1 P1 87.38(7) 2 2 ? C2 Fe1 P1 92.90(7) . 2 ? C1 Fe1 P1 89.721(17) . 2 ? C2 Fe1 P1 92.90(7) 2 . ? C2 Fe1 P1 87.38(7) . . ? C1 Fe1 P1 89.721(17) . . ? P1 Fe1 P1 179.44(3) 2 . ? C11 P1 C21 101.94(9) . . ? C11 P1 C31 102.44(10) . . ? C21 P1 C31 101.63(9) . . ? C11 P1 Fe1 116.00(7) . . ? C21 P1 Fe1 118.04(6) . . ? C31 P1 Fe1 114.49(7) . . ? C32 N1 C31 123.52(19) . . ? C32 N2 C36 116.6(2) . . ? O1 C1 Fe1 180.0 . . ? O2 C2 Fe1 178.4(2) . . ? C16 C11 C12 118.9(2) . . ? C16 C11 P1 118.15(17) . . ? C12 C11 P1 122.92(18) . . ? C11 C12 C13 120.0(3) . . ? C14 C13 C12 120.6(3) . . ? C13 C14 C15 120.1(3) . . ? C14 C15 C16 119.8(3) . . ? C11 C16 C15 120.5(3) . . ? C26 C21 C22 118.69(18) . . ? C26 C21 P1 121.91(14) . . ? C22 C21 P1 119.38(15) . . ? C23 C22 C21 120.3(2) . . ? C24 C23 C22 120.1(2) . . ? C25 C24 C23 120.1(2) . . ? C24 C25 C26 120.5(2) . . ? C21 C26 C25 120.2(2) . . ? N1 C31 P1 112.10(14) . . ? N2 C32 N1 117.7(2) . . ? N2 C32 C33 122.4(2) . . ? N1 C32 C33 119.9(2) . . ? C34 C33 C32 118.6(2) . . ? C33 C34 C35 120.3(2) . . ? C36 C35 C34 117.6(2) . . ? N2 C36 C35 124.4(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.342 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.053 #=============================================END data_compd3 #compound3 _database_code_CSD 171813 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 Cl2 N4 O8 P2 Pd' _chemical_formula_weight 889.91 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6439(18) _cell_length_b 21.221(4) _cell_length_c 18.761(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.442(4) _cell_angle_gamma 90.00 _cell_volume 3798.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6924 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25481 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.00 _reflns_number_total 9136 _reflns_number_gt 5578 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0521P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9136 _refine_ls_number_parameters 479 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.76761(3) 0.215696(12) 0.463987(14) 0.03508(10) Uani 1 1 d . . . P1 P 0.83211(10) 0.21056(4) 0.58301(5) 0.0355(2) Uani 1 1 d . . . P2 P 0.71643(11) 0.31838(4) 0.45543(5) 0.0369(2) Uani 1 1 d . . . N1 N 0.9560(4) 0.09734(14) 0.56178(17) 0.0478(8) Uani 1 1 d . . . H1A H 1.0135 0.0692 0.5814 0.057 Uiso 1 1 calc R . . N2 N 0.7634(3) 0.11551(13) 0.47124(16) 0.0402(7) Uani 1 1 d . . . N3 N 0.6599(3) 0.30876(14) 0.30929(16) 0.0455(8) Uani 1 1 d . . . H3A H 0.6437 0.3360 0.2751 0.055 Uiso 1 1 calc R . . N4 N 0.7779(3) 0.21426(13) 0.34896(15) 0.0397(7) Uani 1 1 d . . . C1 C 0.7186(4) 0.16657(17) 0.6329(2) 0.0419(9) Uani 1 1 d . . . C2 C 0.7772(5) 0.1347(2) 0.6952(2) 0.0655(13) Uani 1 1 d . . . H2A H 0.8728 0.1375 0.7117 0.079 Uiso 1 1 calc R . . C3 C 0.6915(6) 0.0989(3) 0.7319(3) 0.0835(17) Uani 1 1 d . . . H3B H 0.7296 0.0774 0.7734 0.100 Uiso 1 1 calc R . . C4 C 0.5506(6) 0.0948(2) 0.7079(3) 0.0752(16) Uani 1 1 d . . . H4A H 0.4935 0.0712 0.7335 0.090 Uiso 1 1 calc R . . C6 C 0.5775(4) 0.16080(18) 0.6079(2) 0.0458(9) Uani 1 1 d . . . H6A H 0.5388 0.1806 0.5654 0.055 Uiso 1 1 calc R . . C5 C 0.4937(5) 0.1253(2) 0.6466(3) 0.0601(12) Uani 1 1 d . . . H5A H 0.3980 0.1223 0.6306 0.072 Uiso 1 1 calc R . . C7 C 0.8954(4) 0.27748(16) 0.63800(19) 0.0398(9) Uani 1 1 d . . . C8 C 1.0133(4) 0.31006(18) 0.6235(2) 0.0481(10) Uani 1 1 d . . . H8A H 1.0571 0.2983 0.5845 0.058 Uiso 1 1 calc R . . C9 C 1.0655(5) 0.35976(18) 0.6667(2) 0.0570(11) Uani 1 1 d . . . H9A H 1.1449 0.3811 0.6571 0.068 Uiso 1 1 calc R . . C10 C 1.0004(6) 0.3777(2) 0.7237(2) 0.0669(13) Uani 1 1 d . . . H10A H 1.0351 0.4116 0.7523 0.080 Uiso 1 1 calc R . . C11 C 0.8846(6) 0.3459(2) 0.7386(3) 0.0730(15) Uani 1 1 d . . . H11A H 0.8416 0.3581 0.7776 0.088 Uiso 1 1 calc R . . C12 C 0.8306(5) 0.2956(2) 0.6961(2) 0.0598(12) Uani 1 1 d . . . H12A H 0.7518 0.2742 0.7065 0.072 Uiso 1 1 calc R . . C13 C 0.9895(4) 0.16205(17) 0.5810(2) 0.0448(9) Uani 1 1 d . . . H13A H 1.0442 0.1799 0.5465 0.054 Uiso 1 1 calc R . . H13B H 1.0465 0.1632 0.6281 0.054 Uiso 1 1 calc R . . C14 C 0.8441(4) 0.07644(17) 0.5164(2) 0.0424(9) Uani 1 1 d . . . C15 C 0.8111(5) 0.01134(18) 0.5175(2) 0.0570(12) Uani 1 1 d . . . H15A H 0.8681 -0.0159 0.5478 0.068 Uiso 1 1 calc R . . C16 C 0.6974(6) -0.01109(19) 0.4749(3) 0.0711(14) Uani 1 1 d . . . H16A H 0.6756 -0.0537 0.4761 0.085 Uiso 1 1 calc R . . C17 C 0.6110(5) 0.02964(19) 0.4285(2) 0.0637(13) Uani 1 1 d . . . H17A H 0.5320 0.0149 0.3988 0.076 Uiso 1 1 calc R . . C18 C 0.6480(5) 0.09151(18) 0.4290(2) 0.0506(10) Uani 1 1 d . . . H18A H 0.5916 0.1190 0.3990 0.061 Uiso 1 1 calc R . . C19 C 0.6198(4) 0.35644(16) 0.51936(19) 0.0415(9) Uani 1 1 d . . . C20 C 0.6808(5) 0.4000(2) 0.5694(2) 0.0618(12) Uani 1 1 d . . . H20A H 0.7762 0.4084 0.5734 0.074 Uiso 1 1 calc R . . C21 C 0.6000(6) 0.4306(2) 0.6130(3) 0.0713(14) Uani 1 1 d . . . H21A H 0.6410 0.4599 0.6466 0.086 Uiso 1 1 calc R . . C22 C 0.4588(6) 0.4184(2) 0.6074(3) 0.0697(14) Uani 1 1 d . . . H22A H 0.4037 0.4403 0.6358 0.084 Uiso 1 1 calc R . . C23 C 0.4004(6) 0.3739(3) 0.5602(3) 0.0836(17) Uani 1 1 d . . . H23A H 0.3055 0.3646 0.5572 0.100 Uiso 1 1 calc R . . C24 C 0.4811(5) 0.3425(2) 0.5165(2) 0.0659(13) Uani 1 1 d . . . H24A H 0.4405 0.3117 0.4849 0.079 Uiso 1 1 calc R . . C25 C 0.8564(4) 0.37016(16) 0.43890(19) 0.0393(9) Uani 1 1 d . . . C26 C 0.8339(5) 0.43400(18) 0.4294(2) 0.0574(11) Uani 1 1 d . . . H26A H 0.7471 0.4514 0.4337 0.069 Uiso 1 1 calc R . . C27 C 0.9425(6) 0.4720(2) 0.4132(2) 0.0688(14) Uani 1 1 d . . . H27A H 0.9285 0.5151 0.4069 0.083 Uiso 1 1 calc R . . C28 C 1.0692(6) 0.4464(2) 0.4063(3) 0.0736(15) Uani 1 1 d . . . H28A H 1.1415 0.4725 0.3964 0.088 Uiso 1 1 calc R . . C29 C 1.0921(5) 0.3829(2) 0.4138(3) 0.0691(13) Uani 1 1 d . . . H29A H 1.1783 0.3657 0.4077 0.083 Uiso 1 1 calc R . . C30 C 0.9856(4) 0.34485(19) 0.4304(2) 0.0513(10) Uani 1 1 d . . . H30A H 1.0005 0.3017 0.4360 0.062 Uiso 1 1 calc R . . C31 C 0.5900(4) 0.31776(18) 0.3708(2) 0.0441(9) Uani 1 1 d . . . H31A H 0.5225 0.2842 0.3728 0.053 Uiso 1 1 calc R . . H31B H 0.5393 0.3574 0.3660 0.053 Uiso 1 1 calc R . . C32 C 0.7496(4) 0.26101(16) 0.30003(19) 0.0384(9) Uani 1 1 d . . . C33 C 0.8159(5) 0.26258(19) 0.2377(2) 0.0508(11) Uani 1 1 d . . . H33A H 0.7974 0.2957 0.2052 0.061 Uiso 1 1 calc R . . C34 C 0.9054(5) 0.2167(2) 0.2249(2) 0.0602(12) Uani 1 1 d . . . H34A H 0.9499 0.2184 0.1842 0.072 Uiso 1 1 calc R . . C35 C 0.9309(5) 0.1668(2) 0.2730(2) 0.0582(12) Uani 1 1 d . . . H35A H 0.9899 0.1338 0.2646 0.070 Uiso 1 1 calc R . . C36 C 0.8668(4) 0.16780(18) 0.3329(2) 0.0492(10) Uani 1 1 d . . . H36A H 0.8846 0.1345 0.3652 0.059 Uiso 1 1 calc R . . Cl1 Cl 0.63507(11) 0.47467(4) 0.23016(5) 0.0498(3) Uani 1 1 d D . . O1 O 0.6868(4) 0.41712(13) 0.20433(17) 0.0719(9) Uani 1 1 d D . . O2 O 0.7463(4) 0.51396(14) 0.25987(18) 0.0800(10) Uani 1 1 d D . . O3 O 0.5526(4) 0.45772(16) 0.28482(19) 0.0868(11) Uani 1 1 d D . . O4 O 0.5494(4) 0.50504(14) 0.17249(18) 0.0931(13) Uani 1 1 d D . . Cl2 Cl 0.26547(14) 0.19839(6) 0.43438(8) 0.0716(3) Uani 1 1 d D . . O5 O 0.4129(4) 0.1941(2) 0.4376(2) 0.1167(15) Uani 1 1 d D . . O6 O 0.2398(6) 0.2259(3) 0.4991(3) 0.156(2) Uani 1 1 d D . . O7 O 0.2242(6) 0.2400(2) 0.3761(3) 0.143(2) Uani 1 1 d D . . O8 O 0.2040(7) 0.1405(2) 0.4203(3) 0.189(3) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.04464(19) 0.02788(14) 0.03198(15) 0.00015(11) 0.00319(11) 0.00054(13) P1 0.0375(5) 0.0357(5) 0.0327(5) 0.0005(4) 0.0027(4) -0.0045(4) P2 0.0427(6) 0.0292(5) 0.0383(5) -0.0008(4) 0.0042(4) 0.0026(4) N1 0.047(2) 0.0402(18) 0.053(2) 0.0037(15) -0.0017(17) 0.0099(16) N2 0.051(2) 0.0312(15) 0.0387(17) 0.0016(13) 0.0064(15) 0.0008(15) N3 0.059(2) 0.0406(17) 0.0357(17) 0.0064(13) 0.0020(16) 0.0078(16) N4 0.050(2) 0.0328(15) 0.0359(16) 0.0006(13) 0.0045(14) 0.0002(15) C1 0.047(2) 0.042(2) 0.037(2) -0.0034(16) 0.0091(18) -0.0063(18) C2 0.059(3) 0.083(3) 0.055(3) 0.024(2) 0.011(2) -0.009(3) C3 0.090(4) 0.094(4) 0.071(3) 0.037(3) 0.025(3) -0.005(3) C4 0.086(4) 0.068(3) 0.081(4) 0.003(3) 0.045(3) -0.022(3) C6 0.043(2) 0.048(2) 0.047(2) -0.0109(17) 0.0089(19) -0.0050(19) C5 0.049(3) 0.062(3) 0.074(3) -0.022(2) 0.023(2) -0.022(2) C7 0.044(2) 0.039(2) 0.0348(19) 0.0011(15) -0.0014(16) -0.0035(17) C8 0.049(3) 0.043(2) 0.051(2) 0.0040(18) 0.005(2) -0.0076(19) C9 0.058(3) 0.045(2) 0.065(3) 0.003(2) -0.003(2) -0.018(2) C10 0.088(4) 0.049(3) 0.058(3) -0.015(2) -0.006(3) -0.015(3) C11 0.097(4) 0.069(3) 0.056(3) -0.022(2) 0.020(3) -0.022(3) C12 0.068(3) 0.059(3) 0.055(3) -0.011(2) 0.017(2) -0.021(2) C13 0.040(2) 0.044(2) 0.048(2) 0.0071(17) 0.0005(18) -0.0055(18) C14 0.052(3) 0.038(2) 0.039(2) -0.0006(16) 0.0141(19) 0.0054(18) C15 0.079(3) 0.032(2) 0.058(3) 0.0047(18) 0.002(2) 0.009(2) C16 0.104(4) 0.031(2) 0.075(3) -0.004(2) -0.001(3) -0.010(2) C17 0.079(4) 0.044(2) 0.063(3) -0.008(2) -0.006(3) -0.012(2) C18 0.057(3) 0.040(2) 0.051(2) -0.0042(18) -0.002(2) -0.001(2) C19 0.047(2) 0.038(2) 0.039(2) -0.0010(16) 0.0088(18) 0.0039(18) C20 0.055(3) 0.065(3) 0.066(3) -0.025(2) 0.011(2) -0.006(2) C21 0.084(4) 0.065(3) 0.068(3) -0.031(2) 0.020(3) -0.008(3) C22 0.087(4) 0.068(3) 0.061(3) -0.013(2) 0.033(3) 0.006(3) C23 0.068(4) 0.118(5) 0.073(3) -0.032(3) 0.035(3) -0.016(3) C24 0.068(3) 0.071(3) 0.064(3) -0.024(2) 0.029(3) -0.022(3) C25 0.048(2) 0.0337(18) 0.0350(19) 0.0002(15) 0.0017(17) -0.0017(17) C26 0.062(3) 0.043(2) 0.064(3) 0.001(2) 0.002(2) 0.000(2) C27 0.098(4) 0.040(2) 0.067(3) 0.004(2) 0.009(3) -0.021(3) C28 0.083(4) 0.073(3) 0.068(3) -0.003(3) 0.022(3) -0.033(3) C29 0.063(3) 0.073(3) 0.075(3) -0.002(3) 0.025(3) -0.010(3) C30 0.053(3) 0.046(2) 0.055(3) 0.0045(19) 0.012(2) 0.002(2) C31 0.044(2) 0.039(2) 0.048(2) 0.0015(17) 0.0034(19) 0.0042(18) C32 0.045(2) 0.0345(18) 0.0344(19) -0.0009(15) 0.0017(17) -0.0072(17) C33 0.063(3) 0.047(2) 0.044(2) 0.0077(18) 0.015(2) -0.004(2) C34 0.069(3) 0.064(3) 0.053(3) -0.003(2) 0.026(2) -0.004(3) C35 0.065(3) 0.060(3) 0.053(3) -0.007(2) 0.019(2) 0.006(2) C36 0.063(3) 0.042(2) 0.044(2) -0.0007(17) 0.012(2) 0.005(2) Cl1 0.0576(7) 0.0360(5) 0.0524(6) -0.0076(4) -0.0034(5) -0.0008(5) O1 0.088(3) 0.0448(16) 0.082(2) -0.0122(15) 0.0100(19) 0.0141(16) O2 0.080(3) 0.0614(19) 0.091(2) -0.0108(18) -0.014(2) -0.0298(18) O3 0.095(3) 0.087(2) 0.086(3) -0.019(2) 0.039(2) -0.021(2) O4 0.120(3) 0.0527(19) 0.088(2) -0.0013(17) -0.049(2) 0.016(2) Cl2 0.0542(8) 0.0632(7) 0.0950(10) 0.0024(7) 0.0029(7) -0.0040(6) O5 0.065(3) 0.166(4) 0.117(4) -0.025(3) 0.009(2) 0.029(3) O6 0.138(5) 0.199(6) 0.153(5) -0.038(4) 0.094(4) -0.042(4) O7 0.166(5) 0.099(3) 0.156(5) 0.041(3) 0.003(4) 0.038(3) O8 0.222(6) 0.093(3) 0.222(6) 0.047(4) -0.062(5) -0.082(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 2.131(3) . ? Pd1 N4 2.175(3) . ? Pd1 P1 2.2310(10) . ? Pd1 P2 2.2349(10) . ? P1 C1 1.802(4) . ? P1 C7 1.808(4) . ? P1 C13 1.839(4) . ? P2 C25 1.802(4) . ? P2 C19 1.813(4) . ? P2 C31 1.855(4) . ? N1 C14 1.348(5) . ? N1 C13 1.444(4) . ? N2 C14 1.348(5) . ? N2 C18 1.366(5) . ? N3 C32 1.360(5) . ? N3 C31 1.432(4) . ? N4 C32 1.352(4) . ? N4 C36 1.369(5) . ? C1 C6 1.378(5) . ? C1 C2 1.396(5) . ? C2 C3 1.379(6) . ? C3 C4 1.370(7) . ? C4 C5 1.363(7) . ? C6 C5 1.385(5) . ? C7 C12 1.388(5) . ? C7 C8 1.392(5) . ? C8 C9 1.379(5) . ? C9 C10 1.371(6) . ? C10 C11 1.369(6) . ? C11 C12 1.387(6) . ? C14 C15 1.419(5) . ? C15 C16 1.346(6) . ? C16 C17 1.409(6) . ? C17 C18 1.360(5) . ? C19 C24 1.363(6) . ? C19 C20 1.385(5) . ? C20 C21 1.374(6) . ? C21 C22 1.375(7) . ? C22 C23 1.359(7) . ? C23 C24 1.381(6) . ? C25 C26 1.380(5) . ? C25 C30 1.387(5) . ? C26 C27 1.390(6) . ? C27 C28 1.359(7) . ? C28 C29 1.370(7) . ? C29 C30 1.377(6) . ? C32 C33 1.413(5) . ? C33 C34 1.347(6) . ? C34 C35 1.390(6) . ? C35 C36 1.359(5) . ? Cl1 O2 1.408(3) . ? Cl1 O4 1.417(3) . ? Cl1 O1 1.431(3) . ? Cl1 O3 1.433(3) . ? Cl2 O8 1.372(4) . ? Cl2 O6 1.402(5) . ? Cl2 O7 1.417(4) . ? Cl2 O5 1.417(4) . ? 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 N2 Pd1 N4 93.06(10) . . ? N2 Pd1 P1 83.83(8) . . ? N4 Pd1 P1 161.05(9) . . ? N2 Pd1 P2 166.22(9) . . ? N4 Pd1 P2 89.09(8) . . ? P1 Pd1 P2 98.37(4) . . ? C1 P1 C7 106.89(17) . . ? C1 P1 C13 106.64(18) . . ? C7 P1 C13 103.95(18) . . ? C1 P1 Pd1 116.35(13) . . ? C7 P1 Pd1 123.64(12) . . ? C13 P1 Pd1 96.70(13) . . ? C25 P2 C19 108.24(17) . . ? C25 P2 C31 105.77(17) . . ? C19 P2 C31 103.43(18) . . ? C25 P2 Pd1 116.34(13) . . ? C19 P2 Pd1 121.09(12) . . ? C31 P2 Pd1 99.50(12) . . ? C14 N1 C13 126.8(3) . . ? C14 N2 C18 118.7(3) . . ? C14 N2 Pd1 129.7(3) . . ? C18 N2 Pd1 110.9(2) . . ? C32 N3 C31 125.9(3) . . ? C32 N4 C36 116.7(3) . . ? C32 N4 Pd1 129.0(2) . . ? C36 N4 Pd1 110.5(2) . . ? C6 C1 C2 120.0(4) . . ? C6 C1 P1 120.9(3) . . ? C2 C1 P1 118.9(3) . . ? C3 C2 C1 119.1(5) . . ? C4 C3 C2 120.5(5) . . ? C5 C4 C3 120.3(4) . . ? C1 C6 C5 119.5(4) . . ? C4 C5 C6 120.5(5) . . ? C12 C7 C8 119.4(4) . . ? C12 C7 P1 120.8(3) . . ? C8 C7 P1 119.7(3) . . ? C9 C8 C7 120.2(4) . . ? C10 C9 C8 120.1(4) . . ? C11 C10 C9 120.2(4) . . ? C10 C11 C12 120.8(4) . . ? C11 C12 C7 119.3(4) . . ? N1 C13 P1 112.5(3) . . ? N2 C14 N1 122.0(3) . . ? N2 C14 C15 119.9(4) . . ? N1 C14 C15 118.1(4) . . ? C16 C15 C14 120.0(4) . . ? C15 C16 C17 120.4(4) . . ? C18 C17 C16 117.2(4) . . ? C17 C18 N2 123.7(4) . . ? C24 C19 C20 119.2(4) . . ? C24 C19 P2 118.3(3) . . ? C20 C19 P2 122.5(3) . . ? C21 C20 C19 119.9(4) . . ? C20 C21 C22 120.5(4) . . ? C23 C22 C21 119.5(4) . . ? C22 C23 C24 120.4(5) . . ? C19 C24 C23 120.5(4) . . ? C26 C25 C30 119.5(4) . . ? C26 C25 P2 120.9(3) . . ? C30 C25 P2 119.4(3) . . ? C25 C26 C27 119.2(4) . . ? C28 C27 C26 120.4(4) . . ? C27 C28 C29 121.1(5) . . ? C28 C29 C30 119.1(5) . . ? C29 C30 C25 120.7(4) . . ? N3 C31 P2 111.3(3) . . ? N4 C32 N3 121.9(3) . . ? N4 C32 C33 120.6(4) . . ? N3 C32 C33 117.5(3) . . ? C34 C33 C32 120.7(4) . . ? C33 C34 C35 119.4(4) . . ? C36 C35 C34 117.8(4) . . ? C35 C36 N4 124.7(4) . . ? O2 Cl1 O4 111.0(2) . . ? O2 Cl1 O1 110.9(2) . . ? O4 Cl1 O1 108.9(2) . . ? O2 Cl1 O3 109.6(2) . . ? O4 Cl1 O3 109.8(3) . . ? O1 Cl1 O3 106.6(2) . . ? O8 Cl2 O6 114.4(4) . . ? O8 Cl2 O7 110.2(3) . . ? O6 Cl2 O7 110.1(3) . . ? O8 Cl2 O5 110.7(3) . . ? O6 Cl2 O5 107.1(3) . . ? O7 Cl2 O5 103.8(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.772 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.110 #==============================================END data_compd4 #compound4 _database_code_CSD 171814 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H19 Cl4 N2 P Pd' _chemical_formula_weight 554.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.703(2) _cell_length_b 10.229(2) _cell_length_c 12.939(3) _cell_angle_alpha 97.913(5) _cell_angle_beta 103.563(4) _cell_angle_gamma 113.954(4) _cell_volume 1101.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7548 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.11 _reflns_number_total 5232 _reflns_number_gt 3574 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0592P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5232 _refine_ls_number_parameters 244 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.23164(4) 0.71230(4) 0.09411(3) 0.03174(12) Uani 1 1 d . . . Cl1 Cl 0.17167(16) 0.80405(14) 0.24102(10) 0.0464(3) Uani 1 1 d . . . Cl2 Cl 0.31253(18) 0.64237(16) -0.04821(11) 0.0545(4) Uani 1 1 d . . . P1 P 0.31302(13) 0.56806(13) 0.18170(10) 0.0321(3) Uani 1 1 d . . . N1 N -0.1592(5) 0.1565(4) -0.0038(3) 0.0372(9) Uani 1 1 d . . . N2 N 0.1041(4) 0.3144(4) 0.0261(3) 0.0371(9) Uani 1 1 d . . . H2B H 0.0725 0.3655 -0.0283 0.045 Uiso 1 1 d R . . C1 C 0.5261(5) 0.6643(5) 0.2510(4) 0.0348(10) Uani 1 1 d . . . C2 C 0.5879(6) 0.7988(6) 0.3252(5) 0.0592(15) Uani 1 1 d . . . H2A H 0.5213 0.8377 0.3408 0.071 Uiso 1 1 calc R . . C3 C 0.7535(7) 0.8775(7) 0.3775(5) 0.0730(19) Uani 1 1 d . . . H3A H 0.7958 0.9688 0.4282 0.088 Uiso 1 1 calc R . . C4 C 0.8527(6) 0.8234(7) 0.3556(5) 0.0558(15) Uani 1 1 d . . . H4A H 0.9619 0.8762 0.3910 0.067 Uiso 1 1 calc R . . C5 C 0.7893(6) 0.6903(7) 0.2808(5) 0.0576(15) Uani 1 1 d . . . H5A H 0.8562 0.6526 0.2639 0.069 Uiso 1 1 calc R . . C6 C 0.6270(6) 0.6106(6) 0.2297(4) 0.0468(12) Uani 1 1 d . . . H6A H 0.5858 0.5188 0.1799 0.056 Uiso 1 1 calc R . . C7 C 0.2211(5) 0.4974(5) 0.2826(4) 0.0368(10) Uani 1 1 d . . . C8 C 0.3042(6) 0.4674(6) 0.3702(4) 0.0545(14) Uani 1 1 d . . . H8A H 0.4109 0.4916 0.3814 0.065 Uiso 1 1 calc R . . C9 C 0.2304(8) 0.4012(8) 0.4421(5) 0.0707(19) Uani 1 1 d . . . H9A H 0.2866 0.3822 0.5020 0.085 Uiso 1 1 calc R . . C10 C 0.0723(8) 0.3647(8) 0.4226(6) 0.077(2) Uani 1 1 d . . . H10A H 0.0220 0.3206 0.4704 0.092 Uiso 1 1 calc R . . C11 C -0.0140(7) 0.3909(7) 0.3350(5) 0.0654(17) Uani 1 1 d . . . H11A H -0.1215 0.3637 0.3231 0.079 Uiso 1 1 calc R . . C12 C 0.0616(6) 0.4590(6) 0.2641(4) 0.0478(12) Uani 1 1 d . . . H12A H 0.0052 0.4785 0.2046 0.057 Uiso 1 1 calc R . . C13 C 0.2716(5) 0.3946(5) 0.0866(4) 0.0382(11) Uani 1 1 d . . . H13A H 0.3319 0.4173 0.0358 0.046 Uiso 1 1 calc R . . H13B H 0.3040 0.3340 0.1281 0.046 Uiso 1 1 calc R . . C14 C -0.0066(6) 0.1967(5) 0.0493(4) 0.0337(10) Uani 1 1 d . . . C15 C 0.0364(7) 0.1193(6) 0.1218(4) 0.0476(13) Uani 1 1 d . . . H15A H 0.1430 0.1494 0.1594 0.057 Uiso 1 1 calc R . . C16 C -0.0804(8) -0.0007(6) 0.1363(5) 0.0560(15) Uani 1 1 d . . . H16A H -0.0541 -0.0529 0.1843 0.067 Uiso 1 1 calc R . . C17 C -0.2392(7) -0.0445(6) 0.0789(5) 0.0593(16) Uani 1 1 d . . . H17A H -0.3203 -0.1269 0.0869 0.071 Uiso 1 1 calc R . . C18 C -0.2732(7) 0.0370(6) 0.0101(5) 0.0515(13) Uani 1 1 d . . . H18A H -0.3791 0.0085 -0.0282 0.062 Uiso 1 1 calc R . . C19 C 0.5141(15) 0.8375(13) -0.3724(8) 0.186(6) Uani 1 1 d D . . H19A H 0.5659 0.7895 -0.4071 0.224 Uiso 1 1 calc R . . H19B H 0.5885 0.9420 -0.3436 0.224 Uiso 1 1 calc R . . Cl3 Cl 0.4805(4) 0.7703(4) -0.2700(3) 0.1665(13) Uani 1 1 d D . . Cl4 Cl 0.3470(3) 0.8192(3) -0.4742(2) 0.1142(8) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02578(18) 0.03170(19) 0.0362(2) 0.00886(14) 0.00794(14) 0.01274(14) Cl1 0.0510(8) 0.0521(7) 0.0479(7) 0.0144(6) 0.0231(6) 0.0304(6) Cl2 0.0691(9) 0.0691(9) 0.0464(8) 0.0198(7) 0.0276(7) 0.0449(8) P1 0.0239(6) 0.0328(6) 0.0370(7) 0.0090(5) 0.0063(5) 0.0123(5) N1 0.034(2) 0.033(2) 0.045(2) 0.0152(17) 0.0114(18) 0.0149(18) N2 0.030(2) 0.033(2) 0.043(2) 0.0121(17) 0.0045(17) 0.0114(17) C1 0.026(2) 0.037(3) 0.033(2) 0.0097(19) 0.0031(19) 0.011(2) C2 0.036(3) 0.055(3) 0.069(4) -0.006(3) 0.001(3) 0.019(3) C3 0.051(4) 0.054(4) 0.072(5) -0.009(3) -0.006(3) 0.007(3) C4 0.025(3) 0.065(4) 0.061(4) 0.021(3) 0.001(2) 0.011(3) C5 0.032(3) 0.074(4) 0.074(4) 0.028(3) 0.019(3) 0.027(3) C6 0.034(3) 0.047(3) 0.055(3) 0.006(2) 0.013(2) 0.017(2) C7 0.028(2) 0.034(2) 0.044(3) 0.012(2) 0.010(2) 0.011(2) C8 0.034(3) 0.071(4) 0.055(3) 0.032(3) 0.009(2) 0.019(3) C9 0.062(4) 0.096(5) 0.064(4) 0.049(4) 0.024(3) 0.034(4) C10 0.071(5) 0.090(5) 0.082(5) 0.053(4) 0.041(4) 0.029(4) C11 0.044(3) 0.078(4) 0.085(5) 0.037(4) 0.033(3) 0.026(3) C12 0.038(3) 0.056(3) 0.053(3) 0.020(3) 0.019(2) 0.021(3) C13 0.031(2) 0.035(2) 0.047(3) 0.009(2) 0.009(2) 0.015(2) C14 0.039(3) 0.027(2) 0.031(2) 0.0046(18) 0.008(2) 0.013(2) C15 0.046(3) 0.043(3) 0.051(3) 0.017(2) 0.007(2) 0.022(3) C16 0.074(4) 0.046(3) 0.058(4) 0.027(3) 0.027(3) 0.030(3) C17 0.058(4) 0.041(3) 0.087(5) 0.034(3) 0.038(3) 0.017(3) C18 0.045(3) 0.043(3) 0.068(4) 0.017(3) 0.022(3) 0.018(3) C19 0.169(12) 0.133(10) 0.137(10) 0.058(8) -0.019(8) -0.014(8) Cl3 0.128(2) 0.202(3) 0.146(3) 0.091(2) 0.016(2) 0.055(2) Cl4 0.130(2) 0.1102(17) 0.1003(17) 0.0268(13) 0.0276(15) 0.0584(16) _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 2.116(4) 2_565 ? Pd1 P1 2.2520(12) . ? Pd1 Cl2 2.3000(13) . ? Pd1 Cl1 2.3029(13) . ? P1 C1 1.812(5) . ? P1 C7 1.818(5) . ? P1 C13 1.847(5) . ? N1 C14 1.335(6) . ? N1 C18 1.344(6) . ? N1 Pd1 2.116(4) 2_565 ? N2 C14 1.376(5) . ? N2 C13 1.439(6) . ? C1 C6 1.363(6) . ? C1 C2 1.368(7) . ? C2 C3 1.406(7) . ? C3 C4 1.352(8) . ? C4 C5 1.359(8) . ? C5 C6 1.379(7) . ? C7 C8 1.378(7) . ? C7 C12 1.383(6) . ? C8 C9 1.388(7) . ? C9 C10 1.372(9) . ? C10 C11 1.371(8) . ? C11 C12 1.394(7) . ? C14 C15 1.404(6) . ? C15 C16 1.364(7) . ? C16 C17 1.391(8) . ? C17 C18 1.373(7) . ? C19 Cl3 1.614(9) . ? C19 Cl4 1.757(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 N1 Pd1 P1 176.55(11) 2_565 . ? N1 Pd1 Cl2 88.29(11) 2_565 . ? P1 Pd1 Cl2 88.26(5) . . ? N1 Pd1 Cl1 90.16(11) 2_565 . ? P1 Pd1 Cl1 93.29(5) . . ? Cl2 Pd1 Cl1 174.52(5) . . ? C1 P1 C7 106.8(2) . . ? C1 P1 C13 106.7(2) . . ? C7 P1 C13 101.4(2) . . ? C1 P1 Pd1 110.56(15) . . ? C7 P1 Pd1 117.85(16) . . ? C13 P1 Pd1 112.57(16) . . ? C14 N1 C18 119.3(4) . . ? C14 N1 Pd1 122.6(3) . 2_565 ? C18 N1 Pd1 117.7(3) . 2_565 ? C14 N2 C13 126.1(4) . . ? C6 C1 C2 119.0(5) . . ? C6 C1 P1 122.8(4) . . ? C2 C1 P1 118.2(4) . . ? C1 C2 C3 119.1(5) . . ? C4 C3 C2 121.4(6) . . ? C3 C4 C5 118.6(5) . . ? C4 C5 C6 120.8(5) . . ? C1 C6 C5 121.1(5) . . ? C8 C7 C12 120.1(5) . . ? C8 C7 P1 120.4(4) . . ? C12 C7 P1 119.1(4) . . ? C7 C8 C9 120.7(5) . . ? C10 C9 C8 118.3(6) . . ? C11 C10 C9 122.3(5) . . ? C10 C11 C12 119.0(5) . . ? C7 C12 C11 119.6(5) . . ? N2 C13 P1 109.6(3) . . ? N1 C14 N2 116.2(4) . . ? N1 C14 C15 121.2(4) . . ? N2 C14 C15 122.6(4) . . ? C16 C15 C14 119.0(5) . . ? C15 C16 C17 119.7(5) . . ? C18 C17 C16 118.4(5) . . ? N1 C18 C17 122.4(5) . . ? Cl3 C19 Cl4 116.2(8) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.11 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.758 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.109 #==================================================END data_compd5 #compound5 _database_code_CSD 171815 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 Cl Cu N4 O4 P2' _chemical_formula_weight 747.60 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 15.2545(13) _cell_length_b 11.3123(9) _cell_length_c 20.6784(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3568.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8322 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23691 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.00 _reflns_number_total 8170 _reflns_number_gt 6619 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0358P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00058(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(7) _refine_ls_number_reflns 8170 _refine_ls_number_parameters 434 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.516737(17) 0.62923(2) 0.190522(13) 0.03996(7) Uani 1 1 d . . . P1 P 0.47940(4) 0.58307(5) 0.08945(3) 0.04003(13) Uani 1 1 d . . . P2 P 0.53215(4) 0.80804(5) 0.23510(3) 0.04070(13) Uani 1 1 d . . . N1 N 0.37811(15) 0.40914(18) 0.14626(10) 0.0538(6) Uani 1 1 d . . . H1A H 0.3723 0.3409 0.1285 0.065 Uiso 1 1 calc R . . N2 N 0.42321(13) 0.51296(16) 0.23764(9) 0.0448(4) Uani 1 1 d . . . N3 N 0.63318(14) 0.68032(17) 0.32192(10) 0.0522(5) Uani 1 1 d . . . H3A H 0.6221 0.6850 0.3626 0.063 Uiso 1 1 calc R . . N4 N 0.62764(13) 0.55072(16) 0.23417(9) 0.0457(4) Uani 1 1 d . . . C1 C 0.53826(15) 0.47689(18) 0.03925(11) 0.0414(5) Uani 1 1 d . . . C2 C 0.49713(19) 0.3846(3) 0.00727(16) 0.0686(9) Uani 1 1 d . . . H2A H 0.4367 0.3755 0.0108 0.082 Uiso 1 1 calc R . . C3 C 0.5450(2) 0.3055(3) -0.02995(17) 0.0761(9) Uani 1 1 d . . . H3B H 0.5165 0.2443 -0.0514 0.091 Uiso 1 1 calc R . . C4 C 0.6334(2) 0.3169(2) -0.03526(13) 0.0610(7) Uani 1 1 d . . . H4A H 0.6653 0.2629 -0.0596 0.073 Uiso 1 1 calc R . . C5 C 0.67515(19) 0.4077(2) -0.00481(14) 0.0600(7) Uani 1 1 d . . . H5A H 0.7355 0.4163 -0.0092 0.072 Uiso 1 1 calc R . . C6 C 0.62788(17) 0.4879(2) 0.03289(12) 0.0507(6) Uani 1 1 d . . . H6A H 0.6570 0.5490 0.0539 0.061 Uiso 1 1 calc R . . C7 C 0.44570(16) 0.6999(2) 0.03407(12) 0.0482(6) Uani 1 1 d . . . C8 C 0.4380(2) 0.6846(3) -0.03183(14) 0.0758(9) Uani 1 1 d . . . H8A H 0.4513 0.6117 -0.0502 0.091 Uiso 1 1 calc R . . C9 C 0.4107(3) 0.7765(3) -0.07083(16) 0.0930(11) Uani 1 1 d . . . H9A H 0.4076 0.7654 -0.1153 0.112 Uiso 1 1 calc R . . C10 C 0.3885(2) 0.8815(3) -0.04576(19) 0.0863(11) Uani 1 1 d . . . H10A H 0.3692 0.9419 -0.0727 0.104 Uiso 1 1 calc R . . C11 C 0.3943(3) 0.9001(3) 0.0197(2) 0.1019(14) Uani 1 1 d . . . H11A H 0.3788 0.9727 0.0375 0.122 Uiso 1 1 calc R . . C12 C 0.4238(3) 0.8082(3) 0.05898(16) 0.0897(11) Uani 1 1 d . . . H12A H 0.4288 0.8208 0.1033 0.108 Uiso 1 1 calc R . . C13 C 0.37245(16) 0.5120(2) 0.10545(12) 0.0491(6) Uani 1 1 d . . . H13A H 0.3339 0.5692 0.1257 0.059 Uiso 1 1 calc R . . H13B H 0.3463 0.4894 0.0645 0.059 Uiso 1 1 calc R . . C14 C 0.39220(16) 0.4132(2) 0.21135(12) 0.0464(6) Uani 1 1 d . . . C15 C 0.37207(19) 0.3125(2) 0.24948(16) 0.0651(8) Uani 1 1 d . . . H15A H 0.3529 0.2427 0.2303 0.078 Uiso 1 1 calc R . . C16 C 0.42968(17) 0.5158(3) 0.30323(13) 0.0594(7) Uani 1 1 d . . . H16A H 0.4495 0.5853 0.3223 0.071 Uiso 1 1 calc R . . C17 C 0.4092(2) 0.4242(3) 0.34267(15) 0.0703(8) Uani 1 1 d . . . H17A H 0.4138 0.4315 0.3873 0.084 Uiso 1 1 calc R . . C18 C 0.3815(2) 0.3206(3) 0.31492(17) 0.0757(9) Uani 1 1 d . . . H18A H 0.3692 0.2555 0.3409 0.091 Uiso 1 1 calc R . . C19 C 0.56497(16) 0.93594(19) 0.18644(13) 0.0511(5) Uani 1 1 d . . . C20 C 0.53294(18) 1.0485(2) 0.19600(18) 0.0680(8) Uani 1 1 d . . . H20A H 0.4925 1.0620 0.2289 0.082 Uiso 1 1 calc R . . C21 C 0.5599(3) 1.1418(3) 0.1575(2) 0.0937(12) Uani 1 1 d . . . H21A H 0.5361 1.2167 0.1635 0.112 Uiso 1 1 calc R . . C22 C 0.6210(3) 1.1237(3) 0.1112(2) 0.1086(15) Uani 1 1 d . . . H22A H 0.6408 1.1868 0.0864 0.130 Uiso 1 1 calc R . . C23 C 0.6537(3) 1.0126(4) 0.1008(2) 0.1206(16) Uani 1 1 d . . . H23A H 0.6956 1.0007 0.0688 0.145 Uiso 1 1 calc R . . C24 C 0.6251(3) 0.9186(3) 0.13723(17) 0.0875(12) Uani 1 1 d . . . H24A H 0.6462 0.8430 0.1288 0.105 Uiso 1 1 calc R . . C25 C 0.44936(17) 0.87100(18) 0.28863(12) 0.0459(5) Uani 1 1 d . . . C26 C 0.36503(19) 0.8715(2) 0.26633(16) 0.0707(8) Uani 1 1 d . . . H26A H 0.3517 0.8334 0.2277 0.085 Uiso 1 1 calc R . . C27 C 0.2986(2) 0.9284(3) 0.3008(2) 0.0919(12) Uani 1 1 d . . . H27A H 0.2416 0.9287 0.2849 0.110 Uiso 1 1 calc R . . C28 C 0.3172(2) 0.9831(2) 0.35727(18) 0.0805(10) Uani 1 1 d . . . H28A H 0.2732 1.0224 0.3798 0.097 Uiso 1 1 calc R . . C29 C 0.4013(3) 0.9807(3) 0.38150(15) 0.0761(9) Uani 1 1 d . . . H29A H 0.4136 1.0161 0.4210 0.091 Uiso 1 1 calc R . . C30 C 0.4675(2) 0.9255(2) 0.34704(14) 0.0605(7) Uani 1 1 d . . . H30A H 0.5244 0.9250 0.3632 0.073 Uiso 1 1 calc R . . C31 C 0.63281(16) 0.78721(19) 0.28355(13) 0.0503(6) Uani 1 1 d . . . H31A H 0.6828 0.7858 0.2546 0.060 Uiso 1 1 calc R . . H31B H 0.6398 0.8545 0.3121 0.060 Uiso 1 1 calc R . . C32 C 0.65057(15) 0.5718(2) 0.29548(11) 0.0446(5) Uani 1 1 d . . . C33 C 0.6921(2) 0.4850(3) 0.33298(14) 0.0661(7) Uani 1 1 d . . . H33A H 0.7050 0.4992 0.3762 0.079 Uiso 1 1 calc R . . C34 C 0.7132(2) 0.3805(3) 0.30551(16) 0.0793(10) Uani 1 1 d . . . H34A H 0.7420 0.3230 0.3296 0.095 Uiso 1 1 calc R . . C35 C 0.6921(2) 0.3588(2) 0.24194(17) 0.0752(9) Uani 1 1 d . . . H35A H 0.7066 0.2874 0.2223 0.090 Uiso 1 1 calc R . . C36 C 0.64969(18) 0.4446(2) 0.20900(12) 0.0582(7) Uani 1 1 d . . . H36A H 0.6347 0.4297 0.1662 0.070 Uiso 1 1 calc R . . Cl1 Cl 0.72879(4) 0.76578(5) 0.48757(3) 0.05548(16) Uani 1 1 d D . . O1 O 0.71609(16) 0.64691(17) 0.46603(12) 0.0841(6) Uani 1 1 d D . . O2 O 0.70378(18) 0.7732(2) 0.55309(10) 0.1054(9) Uani 1 1 d D . . O3 O 0.67195(18) 0.8359(2) 0.44871(12) 0.0979(7) Uani 1 1 d D . . O4 O 0.81652(16) 0.7998(2) 0.47963(13) 0.1132(9) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.04877(14) 0.03270(12) 0.03842(13) -0.00608(13) -0.00765(16) 0.00233(11) P1 0.0450(3) 0.0394(3) 0.0357(3) -0.0045(2) -0.0051(3) 0.0027(3) P2 0.0486(3) 0.0298(3) 0.0437(3) -0.0063(2) 0.0021(3) 0.0005(2) N1 0.0653(15) 0.0459(12) 0.0502(12) -0.0112(10) 0.0002(10) -0.0128(10) N2 0.0480(11) 0.0455(10) 0.0409(11) -0.0043(9) 0.0033(9) -0.0038(9) N3 0.0623(13) 0.0541(12) 0.0401(11) -0.0117(9) -0.0080(10) 0.0037(10) N4 0.0518(11) 0.0433(10) 0.0420(11) -0.0039(9) -0.0101(9) 0.0084(9) C1 0.0499(14) 0.0393(12) 0.0351(12) -0.0032(9) -0.0032(10) 0.0008(10) C2 0.0532(17) 0.0697(19) 0.083(2) -0.0322(16) 0.0039(14) -0.0101(13) C3 0.078(2) 0.0646(18) 0.086(2) -0.0374(17) 0.0049(17) -0.0107(16) C4 0.075(2) 0.0549(15) 0.0527(16) -0.0093(12) 0.0160(14) 0.0075(14) C5 0.0548(15) 0.0661(16) 0.0591(16) -0.0031(13) 0.0133(13) 0.0011(13) C6 0.0553(16) 0.0517(14) 0.0449(14) -0.0044(11) 0.0026(12) -0.0059(12) C7 0.0474(13) 0.0504(14) 0.0467(14) 0.0007(11) -0.0082(11) 0.0059(11) C8 0.111(3) 0.0694(18) 0.0471(16) 0.0025(14) -0.0013(16) 0.0205(18) C9 0.125(3) 0.102(3) 0.0524(18) 0.0180(18) -0.0082(19) 0.021(2) C10 0.096(3) 0.077(2) 0.086(3) 0.034(2) -0.013(2) 0.0150(19) C11 0.146(4) 0.061(2) 0.099(3) -0.0003(18) -0.027(3) 0.040(2) C12 0.148(3) 0.0612(18) 0.0598(19) -0.0026(16) -0.026(2) 0.034(2) C13 0.0464(14) 0.0572(15) 0.0439(14) -0.0091(11) -0.0043(11) 0.0023(11) C14 0.0416(12) 0.0436(12) 0.0539(14) -0.0035(10) 0.0061(10) -0.0015(11) C15 0.0641(18) 0.0457(14) 0.086(2) 0.0052(14) 0.0106(15) -0.0064(13) C16 0.0605(16) 0.0714(17) 0.0462(15) -0.0042(13) 0.0024(12) -0.0068(14) C17 0.075(2) 0.089(2) 0.0470(16) 0.0122(15) 0.0030(14) -0.0046(17) C18 0.081(2) 0.0705(19) 0.076(2) 0.0320(17) 0.0129(17) 0.0049(17) C19 0.0615(14) 0.0413(11) 0.0507(14) -0.0028(12) 0.0104(14) -0.0028(10) C20 0.081(2) 0.0409(12) 0.082(2) 0.0047(15) 0.0199(19) 0.0045(12) C21 0.119(3) 0.0481(18) 0.114(3) 0.0211(18) 0.022(3) 0.0070(19) C22 0.151(4) 0.070(2) 0.104(3) 0.031(2) 0.036(3) -0.014(2) C23 0.176(4) 0.087(3) 0.099(3) 0.012(2) 0.074(3) -0.011(3) C24 0.124(3) 0.0574(18) 0.081(2) -0.0009(16) 0.049(2) 0.0006(19) C25 0.0549(14) 0.0280(10) 0.0546(14) -0.0034(10) 0.0115(12) -0.0032(10) C26 0.0559(17) 0.0638(17) 0.092(2) -0.0329(16) 0.0107(16) -0.0090(14) C27 0.0572(18) 0.071(2) 0.148(3) -0.038(2) 0.021(2) -0.0048(16) C28 0.082(2) 0.0496(16) 0.110(3) -0.0116(17) 0.048(2) 0.0062(16) C29 0.112(3) 0.0579(17) 0.0587(18) -0.0092(14) 0.0258(18) 0.0144(19) C30 0.0753(19) 0.0544(15) 0.0518(15) -0.0067(13) 0.0072(14) 0.0087(14) C31 0.0518(14) 0.0424(13) 0.0567(15) -0.0117(11) -0.0055(12) -0.0057(11) C32 0.0453(13) 0.0471(13) 0.0414(13) 0.0008(10) -0.0086(10) 0.0002(11) C33 0.080(2) 0.0653(17) 0.0533(16) 0.0054(13) -0.0224(15) 0.0097(15) C34 0.099(2) 0.0592(17) 0.079(2) 0.0074(15) -0.0320(19) 0.0222(17) C35 0.089(2) 0.0543(15) 0.083(2) -0.0079(15) -0.0290(18) 0.0264(15) C36 0.0686(17) 0.0540(14) 0.0519(16) -0.0115(11) -0.0132(12) 0.0216(13) Cl1 0.0696(4) 0.0514(3) 0.0455(3) 0.0042(3) 0.0010(3) -0.0153(3) O1 0.0960(16) 0.0558(11) 0.1005(18) -0.0166(12) -0.0021(13) 0.0021(11) O2 0.151(2) 0.1193(18) 0.0455(12) -0.0021(12) 0.0146(13) -0.0657(17) O3 0.1231(19) 0.0730(13) 0.0977(18) 0.0207(12) -0.0041(16) 0.0216(14) O4 0.0897(18) 0.149(2) 0.1013(19) 0.0132(18) 0.0025(15) -0.0640(17) _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 Cu1 N4 2.1132(18) . ? Cu1 N2 2.1713(19) . ? Cu1 P1 2.2282(6) . ? Cu1 P2 2.2353(6) . ? P1 C7 1.823(2) . ? P1 C1 1.824(2) . ? P1 C13 1.849(2) . ? P2 C25 1.824(2) . ? P2 C19 1.832(2) . ? P2 C31 1.849(3) . ? N1 C14 1.364(3) . ? N1 C13 1.440(3) . ? N2 C14 1.339(3) . ? N2 C16 1.360(3) . ? N3 C32 1.369(3) . ? N3 C31 1.446(3) . ? N4 C32 1.337(3) . ? N4 C36 1.351(3) . ? C1 C6 1.379(3) . ? C1 C2 1.386(3) . ? C2 C3 1.388(4) . ? C3 C4 1.358(4) . ? C4 C5 1.363(4) . ? C5 C6 1.396(4) . ? C7 C12 1.370(4) . ? C7 C8 1.379(4) . ? C8 C9 1.381(4) . ? C9 C10 1.339(5) . ? C10 C11 1.372(5) . ? C11 C12 1.394(4) . ? C14 C15 1.419(4) . ? C15 C18 1.364(4) . ? C16 C17 1.355(4) . ? C17 C18 1.372(4) . ? C19 C20 1.378(3) . ? C19 C24 1.384(4) . ? C20 C21 1.384(4) . ? C21 C22 1.351(5) . ? C22 C23 1.369(5) . ? C23 C24 1.375(4) . ? C25 C26 1.367(4) . ? C25 C30 1.384(4) . ? C26 C27 1.396(4) . ? C27 C28 1.351(5) . ? C28 C29 1.377(5) . ? C29 C30 1.385(4) . ? C32 C33 1.403(3) . ? C33 C34 1.350(4) . ? C34 C35 1.375(4) . ? C35 C36 1.351(4) . ? Cl1 O4 1.402(2) . ? Cl1 O2 1.410(2) . ? Cl1 O3 1.424(2) . ? Cl1 O1 1.430(2) . ? 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 N4 Cu1 N2 94.58(7) . . ? N4 Cu1 P1 120.45(5) . . ? N2 Cu1 P1 96.37(5) . . ? N4 Cu1 P2 96.89(5) . . ? N2 Cu1 P2 115.61(5) . . ? P1 Cu1 P2 128.74(3) . . ? C7 P1 C1 105.00(11) . . ? C7 P1 C13 100.30(11) . . ? C1 P1 C13 104.47(11) . . ? C7 P1 Cu1 119.43(8) . . ? C1 P1 Cu1 124.22(8) . . ? C13 P1 Cu1 99.19(8) . . ? C25 P2 C19 102.36(10) . . ? C25 P2 C31 107.22(12) . . ? C19 P2 C31 99.86(11) . . ? C25 P2 Cu1 122.06(7) . . ? C19 P2 Cu1 121.13(9) . . ? C31 P2 Cu1 101.27(7) . . ? C14 N1 C13 124.1(2) . . ? C14 N2 C16 116.8(2) . . ? C14 N2 Cu1 124.09(15) . . ? C16 N2 Cu1 112.68(16) . . ? C32 N3 C31 122.1(2) . . ? C32 N4 C36 117.3(2) . . ? C32 N4 Cu1 122.65(15) . . ? C36 N4 Cu1 114.09(15) . . ? C6 C1 C2 118.1(2) . . ? C6 C1 P1 118.88(17) . . ? C2 C1 P1 123.02(19) . . ? C1 C2 C3 120.8(3) . . ? C4 C3 C2 120.4(3) . . ? C3 C4 C5 119.9(3) . . ? C4 C5 C6 120.4(3) . . ? C1 C6 C5 120.4(2) . . ? C12 C7 C8 117.6(2) . . ? C12 C7 P1 118.7(2) . . ? C8 C7 P1 123.6(2) . . ? C7 C8 C9 120.5(3) . . ? C10 C9 C8 121.2(3) . . ? C9 C10 C11 120.1(3) . . ? C10 C11 C12 118.8(3) . . ? C7 C12 C11 121.7(3) . . ? N1 C13 P1 113.78(17) . . ? N2 C14 N1 119.0(2) . . ? N2 C14 C15 121.8(2) . . ? N1 C14 C15 119.2(2) . . ? C18 C15 C14 118.3(3) . . ? C17 C16 N2 124.5(3) . . ? C16 C17 C18 118.2(3) . . ? C15 C18 C17 120.3(3) . . ? C20 C19 C24 118.1(3) . . ? C20 C19 P2 123.6(2) . . ? C24 C19 P2 118.2(2) . . ? C19 C20 C21 121.1(3) . . ? C22 C21 C20 119.8(3) . . ? C21 C22 C23 120.1(3) . . ? C22 C23 C24 120.6(4) . . ? C23 C24 C19 120.2(3) . . ? C26 C25 C30 118.8(2) . . ? C26 C25 P2 116.7(2) . . ? C30 C25 P2 124.4(2) . . ? C25 C26 C27 120.8(3) . . ? C28 C27 C26 120.0(3) . . ? C27 C28 C29 120.0(3) . . ? C28 C29 C30 120.1(3) . . ? C25 C30 C29 120.2(3) . . ? N3 C31 P2 114.03(16) . . ? N4 C32 N3 119.2(2) . . ? N4 C32 C33 121.2(2) . . ? N3 C32 C33 119.6(2) . . ? C34 C33 C32 119.2(3) . . ? C33 C34 C35 120.2(3) . . ? C36 C35 C34 117.7(3) . . ? N4 C36 C35 124.3(2) . . ? O4 Cl1 O2 110.76(16) . . ? O4 Cl1 O3 111.23(16) . . ? O2 Cl1 O3 110.15(17) . . ? O4 Cl1 O1 110.56(17) . . ? O2 Cl1 O1 108.58(14) . . ? O3 Cl1 O1 105.40(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.230 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.038 #================================================END data_compd6 #compound6 _database_code_CSD 171816 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 Ag Cl N3 O4 P' _chemical_formula_weight 540.68 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 11.163(3) _cell_length_b 17.485(4) _cell_length_c 11.486(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.452(5) _cell_angle_gamma 90.00 _cell_volume 2241.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.756527 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15419 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.03 _reflns_number_total 7134 _reflns_number_gt 4771 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0783P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(5) _refine_ls_number_reflns 7134 _refine_ls_number_parameters 558 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.04226(6) 0.21850(4) 0.33980(6) 0.0664(2) Uani 1 1 d . . . Ag2 Ag 0.08496(6) 0.29666(4) 0.84946(6) 0.0621(2) Uani 1 1 d . . . P1 P 0.25505(18) 0.33080(11) 0.96553(18) 0.0425(4) Uani 1 1 d . . . P2 P 0.12603(19) 0.12339(11) 0.46283(19) 0.0474(5) Uani 1 1 d . . . N1 N -0.0468(6) 0.2825(3) 1.1990(6) 0.0498(16) Uani 1 1 d . . . N2 N 0.1259(6) 0.3498(4) 1.1600(6) 0.0508(16) Uani 1 1 d . . . H2A H 0.1545 0.3327 1.2251 0.061 Uiso 1 1 calc R . . N3 N -0.0408(6) 0.2945(4) 0.6997(6) 0.0492(16) Uani 1 1 d . . . N4 N 0.0137(6) 0.1719(4) 0.6597(6) 0.0489(15) Uani 1 1 d . . . H4A H 0.0528 0.1734 0.7252 0.059 Uiso 1 1 calc R . . N5 N 0.1251(11) 0.3425(5) 0.4379(9) 0.092(3) Uani 1 1 d . . . N6 N 0.0071(10) 0.1735(6) 0.9388(10) 0.095(3) Uani 1 1 d . . . C1 C 0.3311(7) 0.2537(4) 1.0397(7) 0.0445(17) Uani 1 1 d . . . C2 C 0.4129(9) 0.2661(5) 1.1336(9) 0.063(2) Uani 1 1 d . . . H2B H 0.4285 0.3159 1.1578 0.076 Uiso 1 1 calc R . . C3 C 0.4692(9) 0.2080(6) 1.1892(10) 0.072(3) Uani 1 1 d . . . H3A H 0.5238 0.2178 1.2499 0.086 Uiso 1 1 calc R . . C4 C 0.4452(10) 0.1341(8) 1.1557(13) 0.096(4) Uani 1 1 d . . . H4B H 0.4830 0.0937 1.1945 0.116 Uiso 1 1 calc R . . C5 C 0.3669(10) 0.1197(5) 1.0665(13) 0.089(4) Uani 1 1 d . . . H5B H 0.3512 0.0693 1.0451 0.106 Uiso 1 1 calc R . . C6 C 0.3094(8) 0.1785(5) 1.0063(10) 0.063(3) Uani 1 1 d . . . H6A H 0.2570 0.1677 0.9443 0.076 Uiso 1 1 calc R . . C7 C 0.3765(8) 0.3827(4) 0.8996(7) 0.053(2) Uani 1 1 d . . . C8 C 0.3657(12) 0.4622(6) 0.8822(12) 0.088(4) Uani 1 1 d . . . H8A H 0.2971 0.4880 0.9046 0.105 Uiso 1 1 calc R . . C9 C 0.4592(15) 0.5017(7) 0.8311(13) 0.101(4) Uani 1 1 d . . . H9A H 0.4533 0.5545 0.8232 0.122 Uiso 1 1 calc R . . C10 C 0.5550(13) 0.4672(8) 0.7937(13) 0.098(4) Uani 1 1 d . . . H10A H 0.6158 0.4947 0.7589 0.117 Uiso 1 1 calc R . . C11 C 0.5626(12) 0.3923(9) 0.8069(13) 0.108(5) Uani 1 1 d . . . H11A H 0.6293 0.3675 0.7781 0.130 Uiso 1 1 calc R . . C12 C 0.4747(11) 0.3476(7) 0.8626(11) 0.085(3) Uani 1 1 d . . . H12A H 0.4852 0.2953 0.8730 0.102 Uiso 1 1 calc R . . C13 C 0.2060(7) 0.3913(5) 1.0854(7) 0.0490(19) Uani 1 1 d . . . H13A H 0.2753 0.4085 1.1308 0.059 Uiso 1 1 calc R . . H13B H 0.1653 0.4361 1.0540 0.059 Uiso 1 1 calc R . . C14 C 0.0095(7) 0.3365(4) 1.1340(7) 0.0435(17) Uani 1 1 d . . . C15 C -0.0516(7) 0.3735(5) 1.0431(8) 0.059(2) Uani 1 1 d . . . H15A H -0.0127 0.4089 0.9970 0.071 Uiso 1 1 calc R . . C16 C -0.1698(9) 0.3567(6) 1.0229(10) 0.075(3) Uani 1 1 d . . . H16A H -0.2102 0.3791 0.9598 0.090 Uiso 1 1 calc R . . C17 C -0.2312(10) 0.3066(7) 1.0953(13) 0.091(4) Uani 1 1 d . . . H17A H -0.3136 0.2994 1.0880 0.109 Uiso 1 1 calc R . . C18 C -0.1648(9) 0.2695(6) 1.1756(9) 0.063(3) Uani 1 1 d . . . H18A H -0.2024 0.2320 1.2188 0.076 Uiso 1 1 calc R . . C19 C 0.1564(8) 0.0289(5) 0.4050(8) 0.055(2) Uani 1 1 d . . . C20 C 0.1515(11) -0.0359(5) 0.4682(11) 0.080(3) Uani 1 1 d . . . H20A H 0.1259 -0.0345 0.5446 0.096 Uiso 1 1 calc R . . C21 C 0.1847(12) -0.1047(7) 0.4184(15) 0.093(4) Uani 1 1 d . . . H21A H 0.1788 -0.1487 0.4634 0.112 Uiso 1 1 calc R . . C22 C 0.2237(10) -0.1121(8) 0.3128(16) 0.099(5) Uani 1 1 d . . . H22A H 0.2505 -0.1591 0.2858 0.119 Uiso 1 1 calc R . . C23 C 0.2239(14) -0.0491(8) 0.2438(13) 0.109(4) Uani 1 1 d . . . H23A H 0.2444 -0.0532 0.1660 0.131 Uiso 1 1 calc R . . C24 C 0.1929(13) 0.0227(7) 0.2905(11) 0.097(4) Uani 1 1 d . . . H24A H 0.1969 0.0662 0.2443 0.116 Uiso 1 1 calc R . . C25 C 0.2682(8) 0.1531(5) 0.5317(8) 0.052(2) Uani 1 1 d . . . C26 C 0.3103(9) 0.1236(6) 0.6364(8) 0.064(2) Uani 1 1 d . . . H26A H 0.2626 0.0900 0.6775 0.077 Uiso 1 1 calc R . . C27 C 0.4210(9) 0.1430(7) 0.6807(11) 0.081(3) Uani 1 1 d . . . H27A H 0.4501 0.1196 0.7484 0.097 Uiso 1 1 calc R . . C28 C 0.4883(10) 0.1955(8) 0.6272(14) 0.103(4) Uani 1 1 d . . . H28A H 0.5618 0.2105 0.6597 0.124 Uiso 1 1 calc R . . C29 C 0.4463(10) 0.2275(8) 0.5217(14) 0.102(4) Uani 1 1 d . . . H29A H 0.4924 0.2636 0.4837 0.122 Uiso 1 1 calc R . . C30 C 0.3380(9) 0.2057(5) 0.4749(11) 0.076(3) Uani 1 1 d . . . H30A H 0.3111 0.2264 0.4044 0.091 Uiso 1 1 calc R . . C31 C 0.0277(8) 0.1043(4) 0.5877(7) 0.0480(18) Uani 1 1 d . . . H31A H -0.0504 0.0878 0.5586 0.058 Uiso 1 1 calc R . . H31B H 0.0618 0.0633 0.6347 0.058 Uiso 1 1 calc R . . C32 C -0.0563(6) 0.2325(4) 0.6313(7) 0.0434(17) Uani 1 1 d . . . C33 C -0.1409(7) 0.2334(5) 0.5392(8) 0.053(2) Uani 1 1 d . . . H33A H -0.1513 0.1901 0.4930 0.064 Uiso 1 1 calc R . . C34 C -0.2072(8) 0.2962(6) 0.5170(8) 0.064(2) Uani 1 1 d . . . H34A H -0.2619 0.2972 0.4545 0.077 Uiso 1 1 calc R . . C35 C -0.1923(9) 0.3601(6) 0.5900(10) 0.072(3) Uani 1 1 d . . . H35A H -0.2395 0.4035 0.5793 0.087 Uiso 1 1 calc R . . C36 C -0.1087(9) 0.3571(5) 0.6752(9) 0.062(2) Uani 1 1 d . . . H36A H -0.0962 0.4006 0.7205 0.074 Uiso 1 1 calc R . . C37 C 0.1750(11) 0.3775(7) 0.5064(11) 0.085(3) Uani 1 1 d . . . C38 C 0.242(2) 0.4227(12) 0.5863(14) 0.178(10) Uani 1 1 d . . . H38A H 0.3000 0.3911 0.6268 0.267 Uiso 1 1 calc R . . H38B H 0.1896 0.4454 0.6412 0.267 Uiso 1 1 calc R . . H38C H 0.2831 0.4622 0.5450 0.267 Uiso 1 1 calc R . . C39 C -0.0074(9) 0.1170(8) 0.9810(9) 0.076(3) Uani 1 1 d . . . C40 C -0.0276(13) 0.0407(8) 1.0324(17) 0.128(6) Uani 1 1 d . . . H40A H -0.0962 0.0173 0.9950 0.191 Uiso 1 1 calc R . . H40B H -0.0413 0.0460 1.1141 0.191 Uiso 1 1 calc R . . H40C H 0.0417 0.0092 1.0214 0.191 Uiso 1 1 calc R . . Cl1 Cl 0.7369(2) 0.05799(13) -0.6571(2) 0.0664(6) Uani 1 1 d D . . O1 O 0.6597(9) 0.0010(5) -0.6877(10) 0.137(4) Uani 1 1 d D . . O2 O 0.7311(18) 0.0645(11) -0.5355(10) 0.105(6) Uani 0.50 1 d PD . . O3 O 0.704(3) 0.1243(10) -0.708(2) 0.300 Uiso 0.50 1 d PD . . O4 O 0.8524(10) 0.0412(14) -0.679(2) 0.164(13) Uani 0.50 1 d PD . . O2' O 0.6737(14) 0.1197(10) -0.613(2) 0.146(10) Uani 0.50 1 d PD . . O3' O 0.782(3) 0.0868(16) -0.7611(19) 0.300 Uiso 0.50 1 d PD . . O4' O 0.825(2) 0.0378(10) -0.586(3) 0.35(4) Uani 0.50 1 d PD . . Cl2 Cl 0.0203(3) 0.55402(14) -0.1588(3) 0.0799(7) Uani 1 1 d D . . O5 O 0.0800(12) 0.6126(6) -0.2051(14) 0.214(8) Uani 1 1 d D . . O6 O 0.0732(10) 0.4834(4) -0.1688(10) 0.127(3) Uani 1 1 d D . . O7 O -0.1004(8) 0.5537(8) -0.1730(12) 0.186(6) Uani 1 1 d D . . O8 O 0.0433(14) 0.5620(7) -0.0323(9) 0.166(5) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0786(5) 0.0673(4) 0.0534(4) 0.0264(4) 0.0030(4) 0.0074(3) Ag2 0.0585(4) 0.0741(4) 0.0527(4) -0.0162(4) -0.0153(3) -0.0042(3) P1 0.0466(10) 0.0470(10) 0.0336(10) -0.0034(8) -0.0026(8) -0.0083(8) P2 0.0566(12) 0.0484(11) 0.0373(11) 0.0055(9) 0.0014(9) 0.0035(9) N1 0.063(4) 0.047(4) 0.040(4) 0.006(3) 0.005(3) 0.001(3) N2 0.059(4) 0.063(4) 0.031(4) 0.011(3) 0.000(3) 0.005(3) N3 0.056(4) 0.047(4) 0.044(4) -0.013(3) 0.005(3) -0.003(3) N4 0.058(4) 0.053(4) 0.036(4) -0.007(3) -0.004(3) 0.009(3) N5 0.135(9) 0.075(6) 0.064(6) -0.008(5) -0.013(6) -0.004(6) N6 0.113(8) 0.094(7) 0.078(7) 0.026(6) 0.000(6) -0.039(6) C1 0.041(4) 0.050(4) 0.043(4) 0.001(3) 0.003(3) -0.006(3) C2 0.068(5) 0.055(5) 0.066(6) -0.008(4) -0.014(5) 0.006(4) C3 0.075(6) 0.086(7) 0.055(6) -0.002(5) -0.009(5) 0.019(5) C4 0.072(7) 0.104(9) 0.112(11) 0.047(8) -0.003(7) 0.028(6) C5 0.088(7) 0.051(5) 0.124(11) -0.007(6) -0.033(8) -0.001(5) C6 0.063(5) 0.046(4) 0.080(7) -0.018(5) -0.011(5) 0.000(4) C7 0.065(5) 0.051(4) 0.041(5) 0.007(4) -0.008(4) -0.013(4) C8 0.093(8) 0.077(7) 0.094(10) 0.013(6) 0.017(7) -0.009(6) C9 0.123(11) 0.084(8) 0.099(11) 0.016(7) 0.041(9) -0.042(8) C10 0.095(9) 0.114(10) 0.085(9) 0.034(8) 0.010(7) -0.041(8) C11 0.086(9) 0.138(11) 0.103(11) 0.019(9) 0.050(8) -0.011(8) C12 0.085(8) 0.092(7) 0.079(8) 0.013(6) 0.028(6) 0.004(6) C13 0.053(4) 0.051(4) 0.043(5) 0.003(4) 0.000(4) -0.004(3) C14 0.049(4) 0.044(4) 0.038(4) 0.002(3) -0.004(3) 0.006(3) C15 0.052(5) 0.067(5) 0.058(6) 0.015(4) 0.002(4) 0.012(4) C16 0.069(6) 0.090(7) 0.066(7) 0.034(6) -0.006(5) 0.010(5) C17 0.050(5) 0.116(9) 0.105(11) 0.002(8) -0.007(6) 0.000(6) C18 0.067(6) 0.077(6) 0.046(5) 0.018(5) 0.008(5) -0.019(5) C19 0.051(5) 0.068(5) 0.046(5) -0.008(4) -0.006(4) 0.009(4) C20 0.115(8) 0.050(5) 0.074(7) -0.008(5) -0.012(7) 0.019(5) C21 0.100(9) 0.067(7) 0.114(11) -0.008(7) 0.011(8) 0.008(6) C22 0.067(7) 0.085(8) 0.144(14) -0.063(9) 0.003(8) 0.012(6) C23 0.140(12) 0.113(11) 0.076(9) -0.024(8) 0.021(8) 0.023(9) C24 0.151(11) 0.088(7) 0.052(6) -0.003(6) 0.032(7) 0.028(8) C25 0.060(5) 0.053(4) 0.043(5) 0.008(4) 0.006(4) 0.002(4) C26 0.071(6) 0.075(6) 0.045(5) 0.010(5) -0.008(5) -0.013(5) C27 0.069(6) 0.094(7) 0.078(8) 0.020(6) -0.021(6) -0.001(6) C28 0.057(6) 0.142(11) 0.111(11) 0.012(9) 0.001(7) -0.019(7) C29 0.058(6) 0.126(10) 0.121(12) 0.038(9) -0.003(7) -0.020(6) C30 0.067(6) 0.074(6) 0.087(8) 0.023(6) 0.007(6) 0.009(5) C31 0.060(5) 0.043(4) 0.041(4) 0.004(3) 0.000(4) 0.005(3) C32 0.039(4) 0.056(4) 0.036(4) 0.001(3) 0.000(3) -0.001(3) C33 0.051(4) 0.063(5) 0.045(5) -0.004(4) -0.006(4) 0.000(4) C34 0.054(5) 0.095(7) 0.042(5) -0.001(5) -0.009(4) 0.014(5) C35 0.074(6) 0.079(6) 0.063(7) 0.003(5) -0.002(5) 0.036(5) C36 0.073(6) 0.061(5) 0.051(6) -0.002(4) -0.005(5) 0.011(4) C37 0.098(8) 0.096(8) 0.062(7) -0.002(6) 0.007(7) -0.018(7) C38 0.24(2) 0.24(2) 0.062(9) -0.032(12) 0.006(12) -0.140(18) C39 0.058(5) 0.126(9) 0.045(5) 0.000(6) 0.008(4) -0.022(6) C40 0.105(10) 0.116(11) 0.162(16) 0.061(11) 0.024(11) -0.004(8) Cl1 0.0740(15) 0.0684(13) 0.0561(14) -0.0029(11) -0.0107(12) -0.0032(12) O1 0.119(8) 0.147(8) 0.147(11) -0.070(8) 0.017(7) -0.036(7) O2 0.146(17) 0.131(15) 0.038(8) 0.001(9) 0.013(10) 0.002(12) O4 0.041(9) 0.32(4) 0.13(2) -0.07(2) -0.008(11) 0.006(14) O2' 0.109(13) 0.151(17) 0.18(2) -0.126(18) -0.051(14) 0.046(13) O4' 0.40(6) 0.14(2) 0.48(7) -0.18(3) -0.42(6) 0.15(3) Cl2 0.0862(18) 0.0643(13) 0.089(2) 0.0157(14) -0.0057(15) 0.0025(13) O5 0.220(14) 0.151(9) 0.27(2) 0.126(12) -0.041(14) -0.042(10) O6 0.173(10) 0.105(6) 0.102(8) 0.014(6) 0.013(7) 0.028(7) O7 0.096(8) 0.34(2) 0.122(11) 0.023(12) -0.015(8) 0.034(10) O8 0.219(14) 0.192(12) 0.083(8) -0.009(8) -0.045(9) -0.021(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 Ag1 N1 2.185(7) 1_554 ? Ag1 P2 2.360(2) . ? Ag1 N5 2.603(10) . ? Ag2 N3 2.192(7) . ? Ag2 P1 2.369(2) . ? Ag2 N6 2.548(10) . ? P1 C1 1.796(8) . ? P1 C7 1.813(9) . ? P1 C13 1.831(9) . ? P2 C19 1.816(9) . ? P2 C25 1.830(9) . ? P2 C31 1.859(9) . ? N1 C18 1.356(12) . ? N1 C14 1.366(10) . ? N1 Ag1 2.185(7) 1_556 ? N2 C14 1.346(10) . ? N2 C13 1.448(10) . ? N3 C32 1.347(10) . ? N3 C36 1.357(11) . ? N4 C32 1.352(10) . ? N4 C31 1.452(10) . ? N5 C37 1.132(14) . ? N6 C39 1.114(14) . ? C1 C6 1.389(12) . ? C1 C2 1.413(12) . ? C2 C3 1.347(13) . ? C3 C4 1.372(16) . ? C4 C5 1.354(17) . ? C5 C6 1.387(15) . ? C7 C12 1.335(14) . ? C7 C8 1.409(13) . ? C8 C9 1.393(17) . ? C9 C10 1.309(19) . ? C10 C11 1.321(18) . ? C11 C12 1.420(16) . ? C14 C15 1.392(11) . ? C15 C16 1.365(13) . ? C16 C17 1.401(16) . ? C17 C18 1.335(16) . ? C19 C20 1.346(13) . ? C19 C24 1.392(15) . ? C20 C21 1.387(15) . ? C21 C22 1.31(2) . ? C22 C23 1.36(2) . ? C23 C24 1.410(16) . ? C25 C30 1.379(13) . ? C25 C26 1.380(13) . ? C26 C27 1.368(14) . ? C27 C28 1.345(16) . ? C28 C29 1.40(2) . ? C29 C30 1.365(17) . ? C32 C33 1.400(11) . ? C33 C34 1.346(12) . ? C34 C35 1.405(14) . ? C35 C36 1.337(14) . ? C37 C38 1.412(19) . ? C39 C40 1.478(17) . ? Cl1 O4' 1.308(12) . ? Cl1 O3 1.345(14) . ? Cl1 O4 1.353(12) . ? Cl1 O1 1.357(8) . ? Cl1 O2' 1.392(11) . ? Cl1 O3' 1.402(15) . ? Cl1 O2 1.404(11) . ? O2 O4' 1.30(3) . ? O2 O2' 1.45(2) . ? O3 O2' 1.15(3) . ? O3 O3' 1.26(4) . ? O4 O4' 1.12(4) . ? O4 O3' 1.45(4) . ? Cl2 O5 1.339(10) . ? Cl2 O7 1.353(9) . ? Cl2 O6 1.375(8) . ? Cl2 O8 1.476(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 N1 Ag1 P2 165.90(18) 1_554 . ? N1 Ag1 N5 92.5(3) 1_554 . ? P2 Ag1 N5 101.4(2) . . ? N3 Ag2 P1 159.05(19) . . ? N3 Ag2 N6 94.8(3) . . ? P1 Ag2 N6 105.3(2) . . ? C1 P1 C7 103.0(4) . . ? C1 P1 C13 102.9(4) . . ? C7 P1 C13 105.4(4) . . ? C1 P1 Ag2 116.1(3) . . ? C7 P1 Ag2 119.2(3) . . ? C13 P1 Ag2 108.5(3) . . ? C19 P2 C25 104.4(4) . . ? C19 P2 C31 103.8(4) . . ? C25 P2 C31 103.9(4) . . ? C19 P2 Ag1 119.8(3) . . ? C25 P2 Ag1 112.6(3) . . ? C31 P2 Ag1 110.8(3) . . ? C18 N1 C14 117.7(7) . . ? C18 N1 Ag1 118.9(6) . 1_556 ? C14 N1 Ag1 123.4(5) . 1_556 ? C14 N2 C13 124.2(6) . . ? C32 N3 C36 117.7(8) . . ? C32 N3 Ag2 122.8(5) . . ? C36 N3 Ag2 119.5(6) . . ? C32 N4 C31 124.7(7) . . ? C37 N5 Ag1 156.1(10) . . ? C39 N6 Ag2 168.4(10) . . ? C6 C1 C2 117.4(8) . . ? C6 C1 P1 120.2(7) . . ? C2 C1 P1 122.4(6) . . ? C3 C2 C1 122.1(9) . . ? C2 C3 C4 119.5(10) . . ? C5 C4 C3 120.4(10) . . ? C4 C5 C6 121.4(10) . . ? C5 C6 C1 119.3(9) . . ? C12 C7 C8 118.5(10) . . ? C12 C7 P1 122.1(7) . . ? C8 C7 P1 119.4(8) . . ? C9 C8 C7 119.1(12) . . ? C10 C9 C8 122.5(12) . . ? C9 C10 C11 118.0(12) . . ? C10 C11 C12 123.7(13) . . ? C7 C12 C11 118.2(11) . . ? N2 C13 P1 110.9(5) . . ? N2 C14 N1 117.0(7) . . ? N2 C14 C15 122.5(7) . . ? N1 C14 C15 120.5(7) . . ? C16 C15 C14 118.7(8) . . ? C15 C16 C17 121.3(9) . . ? C18 C17 C16 116.3(10) . . ? C17 C18 N1 125.1(9) . . ? C20 C19 C24 117.4(10) . . ? C20 C19 P2 123.9(8) . . ? C24 C19 P2 118.6(8) . . ? C19 C20 C21 119.5(12) . . ? C22 C21 C20 124.6(14) . . ? C21 C22 C23 117.9(11) . . ? C22 C23 C24 119.7(13) . . ? C19 C24 C23 120.6(12) . . ? C30 C25 C26 118.5(9) . . ? C30 C25 P2 118.6(7) . . ? C26 C25 P2 122.9(7) . . ? C27 C26 C25 121.1(9) . . ? C28 C27 C26 120.6(11) . . ? C27 C28 C29 119.2(11) . . ? C30 C29 C28 120.1(11) . . ? C29 C30 C25 120.4(11) . . ? N4 C31 P2 111.6(5) . . ? N3 C32 N4 115.1(7) . . ? N3 C32 C33 120.5(7) . . ? N4 C32 C33 124.4(8) . . ? C34 C33 C32 120.6(8) . . ? C33 C34 C35 118.7(8) . . ? C36 C35 C34 118.4(8) . . ? C35 C36 N3 124.1(9) . . ? N5 C37 C38 176.3(14) . . ? N6 C39 C40 177.8(14) . . ? O4' Cl1 O3 134.1(14) . . ? O4' Cl1 O4 49.8(16) . . ? O3 Cl1 O4 111.0(11) . . ? O4' Cl1 O1 115.2(10) . . ? O3 Cl1 O1 110.8(10) . . ? O4 Cl1 O1 113.2(9) . . ? O4' Cl1 O2' 111.3(10) . . ? O3 Cl1 O2' 49.7(14) . . ? O4 Cl1 O2' 137.0(11) . . ? O1 Cl1 O2' 109.8(8) . . ? O4' Cl1 O3' 110.2(11) . . ? O3 Cl1 O3' 54.7(16) . . ? O4 Cl1 O3' 63.3(17) . . ? O1 Cl1 O3' 106.4(11) . . ? O2' Cl1 O3' 103.2(10) . . ? O4' Cl1 O2 57.1(15) . . ? O3 Cl1 O2 109.9(11) . . ? O4 Cl1 O2 105.9(9) . . ? O1 Cl1 O2 105.8(8) . . ? O2' Cl1 O2 62.5(11) . . ? O3' Cl1 O2 147.6(13) . . ? O4' O2 Cl1 57.7(9) . . ? O4' O2 O2' 108.2(15) . . ? Cl1 O2 O2' 58.3(8) . . ? O2' O3 O3' 130.1(18) . . ? O2' O3 Cl1 67.3(10) . . ? O3' O3 Cl1 64.9(12) . . ? O4' O4 Cl1 63.0(10) . . ? O4' O4 O3' 119.3(16) . . ? Cl1 O4 O3' 60.0(10) . . ? O3 O2' Cl1 63.0(10) . . ? O3 O2' O2 119.5(14) . . ? Cl1 O2' O2 59.2(7) . . ? O3 O3' Cl1 60.3(10) . . ? O3 O3' O4 110.0(17) . . ? Cl1 O3' O4 56.7(10) . . ? O4 O4' O2 130.7(16) . . ? O4 O4' Cl1 67.2(12) . . ? O2 O4' Cl1 65.2(10) . . ? O5 Cl2 O7 117.3(7) . . ? O5 Cl2 O6 115.8(8) . . ? O7 Cl2 O6 114.5(8) . . ? O5 Cl2 O8 104.1(8) . . ? O7 Cl2 O8 105.5(9) . . ? O6 Cl2 O8 96.0(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.011 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.092 #==============================================END data_compd7 #compound7 _database_code_CSD 171817 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H43 Ag Cl N7 O4 P2' _chemical_formula_weight 927.10 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1602(19) _cell_length_b 11.3068(17) _cell_length_c 17.485(3) _cell_angle_alpha 92.014(13) _cell_angle_beta 94.209(15) _cell_angle_gamma 104.595(11) _cell_volume 2126.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.663 _exptl_absorpt_correction_type PSI-SCAN _exptl_absorpt_correction_T_min 0.721 _exptl_absorpt_correction_T_max 0.830 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9709 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8349 _reflns_number_gt 5597 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0670P)^2^+0.9695P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8349 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.77470(4) 0.52118(3) 0.69565(2) 0.05389(14) Uani 1 1 d . . . P1 P 0.88040(12) 0.70540(11) 0.63538(7) 0.0513(3) Uani 1 1 d . . . C1 C 0.8700(5) 0.8481(4) 0.6806(3) 0.0555(12) Uani 1 1 d . . . C2 C 0.9715(6) 0.9466(5) 0.7021(4) 0.0785(17) Uani 1 1 d . . . H2A H 1.0509 0.9416 0.6922 0.094 Uiso 1 1 calc R . . C3 C 0.9559(8) 1.0496(6) 0.7374(5) 0.099(2) Uani 1 1 d . . . H3A H 1.0252 1.1143 0.7512 0.119 Uiso 1 1 calc R . . C4 C 0.8435(8) 1.0609(6) 0.7530(4) 0.099(2) Uani 1 1 d . . . H4A H 0.8350 1.1328 0.7768 0.119 Uiso 1 1 calc R . . C5 C 0.7406(7) 0.9651(7) 0.7336(4) 0.094(2) Uani 1 1 d . . . H5A H 0.6621 0.9714 0.7445 0.112 Uiso 1 1 calc R . . C6 C 0.7555(6) 0.8588(5) 0.6973(3) 0.0733(15) Uani 1 1 d . . . H6A H 0.6861 0.7939 0.6842 0.088 Uiso 1 1 calc R . . C7 C 0.8448(4) 0.7222(5) 0.5340(3) 0.0561(12) Uani 1 1 d . . . C8 C 0.8109(5) 0.6188(6) 0.4849(3) 0.0750(16) Uani 1 1 d . . . H8A H 0.8059 0.5425 0.5046 0.090 Uiso 1 1 calc R . . C9 C 0.7843(6) 0.6266(7) 0.4073(3) 0.093(2) Uani 1 1 d . . . H9A H 0.7633 0.5560 0.3750 0.112 Uiso 1 1 calc R . . C10 C 0.7888(6) 0.7373(9) 0.3778(4) 0.100(2) Uani 1 1 d . . . H10A H 0.7711 0.7427 0.3254 0.120 Uiso 1 1 calc R . . C11 C 0.8191(8) 0.8395(8) 0.4254(4) 0.110(3) Uani 1 1 d . . . H11A H 0.8202 0.9147 0.4052 0.132 Uiso 1 1 calc R . . C12 C 0.8485(6) 0.8349(6) 0.5034(3) 0.0850(19) Uani 1 1 d . . . H12A H 0.8703 0.9063 0.5350 0.102 Uiso 1 1 calc R . . C13 C 1.0489(4) 0.7148(5) 0.6398(3) 0.0598(13) Uani 1 1 d . . . H13A H 1.0621 0.6470 0.6088 0.072 Uiso 1 1 calc R . . H13B H 1.0917 0.7902 0.6181 0.072 Uiso 1 1 calc R . . N1 N 1.1014(4) 0.7114(4) 0.7176(2) 0.0617(11) Uani 1 1 d . . . H1A H 1.1366 0.7797 0.7426 0.074 Uiso 1 1 calc R . . N2 N 1.0321(4) 0.5019(4) 0.7165(2) 0.0608(11) Uani 1 1 d . . . C14 C 1.0979(4) 0.6062(4) 0.7531(3) 0.0517(11) Uani 1 1 d . . . C15 C 1.1627(5) 0.6099(5) 0.8245(3) 0.0684(15) Uani 1 1 d . . . H15A H 1.2057 0.6839 0.8497 0.082 Uiso 1 1 calc R . . C16 C 1.1611(6) 0.5000(6) 0.8568(3) 0.0845(18) Uani 1 1 d . . . H16A H 1.2053 0.4993 0.9039 0.101 Uiso 1 1 calc R . . C17 C 1.0951(7) 0.3922(6) 0.8199(4) 0.0873(19) Uani 1 1 d . . . H17A H 1.0932 0.3175 0.8411 0.105 Uiso 1 1 calc R . . C18 C 1.0328(6) 0.3985(5) 0.7516(3) 0.0765(17) Uani 1 1 d . . . H18A H 0.9867 0.3252 0.7269 0.092 Uiso 1 1 calc R . . P2 P 0.71416(12) 0.50259(11) 0.82732(6) 0.0505(3) Uani 1 1 d . . . C19 C 0.7686(5) 0.6365(4) 0.8934(3) 0.0570(13) Uani 1 1 d . . . C20 C 0.8541(6) 0.7375(5) 0.8716(3) 0.0809(19) Uani 1 1 d . . . H20A H 0.8838 0.7357 0.8234 0.097 Uiso 1 1 calc R . . C21 C 0.8963(8) 0.8405(5) 0.9193(4) 0.113(3) Uani 1 1 d . . . H21A H 0.9545 0.9075 0.9036 0.135 Uiso 1 1 calc R . . C22 C 0.8528(8) 0.8448(6) 0.9901(5) 0.113(3) Uani 1 1 d . . . H22A H 0.8813 0.9150 1.0224 0.135 Uiso 1 1 calc R . . C23 C 0.7672(7) 0.7458(6) 1.0139(4) 0.093(2) Uani 1 1 d . . . H23A H 0.7372 0.7488 1.0620 0.112 Uiso 1 1 calc R . . C24 C 0.7258(6) 0.6409(5) 0.9649(3) 0.0723(16) Uani 1 1 d . . . H24A H 0.6687 0.5732 0.9809 0.087 Uiso 1 1 calc R . . C25 C 0.7492(5) 0.3791(4) 0.8818(2) 0.0558(13) Uani 1 1 d . . . C26 C 0.8496(5) 0.3981(5) 0.9327(3) 0.0744(16) Uani 1 1 d . . . H26A H 0.9017 0.4766 0.9411 0.089 Uiso 1 1 calc R . . C27 C 0.8769(6) 0.3029(5) 0.9730(4) 0.087(2) Uani 1 1 d . . . H27A H 0.9460 0.3187 1.0086 0.105 Uiso 1 1 calc R . . C28 C 0.8054(8) 0.1897(6) 0.9611(4) 0.100(2) Uani 1 1 d . . . H28A H 0.8204 0.1274 0.9908 0.120 Uiso 1 1 calc R . . C29 C 0.7100(8) 0.1657(6) 0.9053(4) 0.108(2) Uani 1 1 d . . . H29A H 0.6641 0.0855 0.8934 0.129 Uiso 1 1 calc R . . C30 C 0.6809(7) 0.2613(5) 0.8659(3) 0.091(2) Uani 1 1 d . . . H30A H 0.6144 0.2447 0.8284 0.109 Uiso 1 1 calc R . . C31 C 0.5427(5) 0.4708(5) 0.8275(3) 0.0644(14) Uani 1 1 d . . . H31A H 0.5046 0.3987 0.7942 0.077 Uiso 1 1 calc R . . H31B H 0.5197 0.4529 0.8791 0.077 Uiso 1 1 calc R . . N3 N 0.4948(4) 0.5701(4) 0.8026(2) 0.0680(12) Uani 1 1 d . . . H3B H 0.4726 0.6141 0.8373 0.082 Uiso 1 1 calc R . . N4 N 0.5216(4) 0.5375(4) 0.6754(2) 0.0594(11) Uani 1 1 d . . . C32 C 0.4814(4) 0.6010(5) 0.7283(3) 0.0568(12) Uani 1 1 d . . . C33 C 0.4284(5) 0.6974(6) 0.7111(4) 0.0772(16) Uani 1 1 d . . . H33A H 0.4012 0.7405 0.7497 0.093 Uiso 1 1 calc R . . C34 C 0.4178(6) 0.7269(6) 0.6365(5) 0.091(2) Uani 1 1 d . . . H34A H 0.3817 0.7898 0.6232 0.109 Uiso 1 1 calc R . . C35 C 0.4611(6) 0.6624(7) 0.5809(4) 0.090(2) Uani 1 1 d . . . H35A H 0.4562 0.6822 0.5298 0.109 Uiso 1 1 calc R . . C36 C 0.5109(6) 0.5695(6) 0.6023(3) 0.0753(16) Uani 1 1 d . . . H36A H 0.5391 0.5258 0.5646 0.090 Uiso 1 1 calc R . . N5 N 0.5304(8) 0.2794(8) 0.6602(5) 0.076(3) Uani 0.585(11) 1 d P . . N5' N 0.9076(10) 0.3599(10) 0.5774(6) 0.067(4) Uani 0.415(11) 1 d P . . N6 N 0.7234(4) 0.3327(4) 0.6242(2) 0.0593(11) Uani 1 1 d . . . C37 C 0.6124(7) 0.2522(5) 0.6299(4) 0.0765(18) Uani 1 1 d . . . C38 C 0.5901(10) 0.1334(7) 0.5962(5) 0.128(4) Uani 1 1 d . . . H38A H 0.5139 0.0773 0.5991 0.153 Uiso 1 1 calc R . . C39 C 0.6824(17) 0.1010(10) 0.5588(6) 0.173(7) Uani 1 1 d . . . H39A H 0.6693 0.0213 0.5383 0.208 Uiso 1 1 calc R . . C40 C 0.7909(13) 0.1823(10) 0.5515(5) 0.140(4) Uani 1 1 d . . . H40A H 0.8512 0.1612 0.5238 0.168 Uiso 1 1 calc R . . C41 C 0.8111(8) 0.2976(6) 0.5858(3) 0.0763(17) Uani 1 1 d . . . Cl1 Cl 1.33079(15) 1.02251(14) 0.78706(11) 0.0871(5) Uani 1 1 d . . . O1 O 1.2952(6) 0.9833(6) 0.7095(3) 0.137(2) Uani 1 1 d . . . O2 O 1.4517(6) 1.0127(7) 0.8036(5) 0.194(3) Uani 1 1 d . . . O3 O 1.2502(8) 0.9440(7) 0.8291(4) 0.191(3) Uani 1 1 d . . . O4 O 1.3237(8) 1.1404(5) 0.7978(4) 0.173(3) Uani 1 1 d . . . N7 N 0.5710(8) 0.3557(10) 1.0358(5) 0.151(3) Uani 1 1 d . . . C42 C 0.5283(10) 0.2492(12) 1.0390(8) 0.154(4) Uani 1 1 d . . . C43 C 0.4742(13) 0.1308(12) 1.0405(12) 0.326(13) Uani 1 1 d . . . H43A H 0.4996 0.1009 1.0882 0.489 Uiso 1 1 calc R . . H43B H 0.4983 0.0874 0.9986 0.489 Uiso 1 1 calc R . . H43C H 0.3856 0.1183 1.0360 0.489 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 Ag1 0.0572(2) 0.0517(2) 0.0456(2) 0.01165(15) 0.00348(16) -0.00018(16) P1 0.0480(7) 0.0525(7) 0.0502(7) 0.0192(5) 0.0036(6) 0.0051(6) C1 0.055(3) 0.049(3) 0.060(3) 0.019(2) 0.003(2) 0.008(2) C2 0.068(4) 0.048(3) 0.117(5) 0.020(3) 0.008(3) 0.009(3) C3 0.098(6) 0.055(4) 0.138(6) 0.009(4) 0.014(5) 0.008(4) C4 0.131(7) 0.057(4) 0.112(5) 0.004(4) 0.026(5) 0.025(4) C5 0.091(5) 0.095(5) 0.105(5) 0.019(4) 0.030(4) 0.034(4) C6 0.076(4) 0.065(4) 0.076(4) 0.007(3) 0.013(3) 0.012(3) C7 0.049(3) 0.071(3) 0.048(3) 0.025(2) 0.008(2) 0.011(2) C8 0.071(4) 0.088(4) 0.058(3) 0.016(3) -0.001(3) 0.006(3) C9 0.087(5) 0.127(6) 0.058(3) 0.011(4) 0.003(3) 0.015(4) C10 0.079(5) 0.169(8) 0.054(4) 0.037(5) 0.008(3) 0.029(5) C11 0.130(7) 0.135(7) 0.081(5) 0.067(5) 0.016(5) 0.052(6) C12 0.105(5) 0.084(4) 0.071(4) 0.034(3) 0.009(3) 0.029(4) C13 0.054(3) 0.061(3) 0.065(3) 0.026(2) 0.008(2) 0.011(2) N1 0.059(3) 0.051(2) 0.066(3) 0.011(2) -0.013(2) 0.002(2) N2 0.073(3) 0.051(2) 0.058(2) 0.0105(19) -0.002(2) 0.016(2) C14 0.048(3) 0.054(3) 0.056(3) 0.013(2) 0.002(2) 0.017(2) C15 0.070(4) 0.065(3) 0.061(3) 0.003(3) -0.014(3) 0.006(3) C16 0.098(5) 0.095(5) 0.061(3) 0.022(3) -0.012(3) 0.029(4) C17 0.116(6) 0.064(4) 0.080(4) 0.020(3) -0.009(4) 0.023(4) C18 0.104(5) 0.052(3) 0.069(3) 0.006(3) -0.003(3) 0.015(3) P2 0.0558(8) 0.0490(7) 0.0376(6) 0.0096(5) -0.0041(5) -0.0019(6) C19 0.067(3) 0.052(3) 0.047(3) 0.009(2) -0.013(2) 0.010(2) C20 0.100(5) 0.063(3) 0.060(3) 0.019(3) -0.027(3) -0.009(3) C21 0.155(7) 0.054(4) 0.095(5) 0.014(3) -0.056(5) -0.018(4) C22 0.166(8) 0.055(4) 0.101(6) -0.013(4) -0.062(6) 0.021(5) C23 0.133(6) 0.086(5) 0.061(3) -0.016(3) -0.025(4) 0.039(5) C24 0.088(4) 0.066(3) 0.057(3) 0.003(3) -0.015(3) 0.015(3) C25 0.074(3) 0.049(3) 0.036(2) 0.0061(19) -0.001(2) 0.000(2) C26 0.071(4) 0.053(3) 0.090(4) 0.015(3) -0.017(3) 0.005(3) C27 0.100(5) 0.069(4) 0.088(4) 0.006(3) -0.032(4) 0.022(4) C28 0.141(7) 0.060(4) 0.094(5) 0.026(3) -0.015(5) 0.018(4) C29 0.135(7) 0.059(4) 0.110(5) 0.015(4) -0.018(5) -0.003(4) C30 0.115(5) 0.061(3) 0.079(4) 0.012(3) -0.028(4) -0.003(4) C31 0.062(3) 0.075(3) 0.045(3) 0.010(2) 0.007(2) -0.003(3) N3 0.059(3) 0.100(4) 0.046(2) -0.007(2) 0.005(2) 0.022(3) N4 0.060(3) 0.067(3) 0.047(2) -0.003(2) -0.010(2) 0.012(2) C32 0.041(3) 0.068(3) 0.056(3) 0.001(2) -0.006(2) 0.007(2) C33 0.057(4) 0.093(4) 0.086(4) 0.008(3) 0.005(3) 0.029(3) C34 0.069(4) 0.092(5) 0.116(6) 0.027(4) -0.005(4) 0.032(4) C35 0.093(5) 0.110(5) 0.067(4) 0.019(4) -0.015(4) 0.027(4) C36 0.081(4) 0.092(4) 0.050(3) 0.001(3) -0.010(3) 0.023(3) N5 0.062(6) 0.074(6) 0.094(6) 0.002(5) 0.018(5) 0.019(4) N5' 0.046(7) 0.070(7) 0.081(8) 0.003(6) 0.011(6) 0.005(6) N6 0.068(3) 0.055(2) 0.051(2) 0.0000(19) -0.005(2) 0.011(2) C37 0.082(5) 0.057(3) 0.073(4) 0.006(3) -0.022(3) -0.006(3) C38 0.163(9) 0.069(5) 0.113(7) 0.019(4) -0.047(6) -0.029(5) C39 0.35(2) 0.087(7) 0.084(6) -0.004(5) -0.015(10) 0.068(10) C40 0.264(15) 0.125(8) 0.072(5) 0.020(6) 0.031(7) 0.118(9) C41 0.109(6) 0.077(4) 0.053(3) 0.003(3) -0.003(3) 0.046(4) Cl1 0.0767(11) 0.0611(9) 0.1098(13) 0.0099(8) -0.0218(9) 0.0000(8) O1 0.133(5) 0.150(5) 0.119(4) -0.012(4) -0.016(4) 0.029(4) O2 0.106(5) 0.209(7) 0.255(9) -0.027(6) -0.077(5) 0.050(5) O3 0.212(8) 0.156(6) 0.153(6) 0.056(5) 0.009(5) -0.055(5) O4 0.249(9) 0.088(4) 0.184(6) -0.004(4) 0.001(6) 0.055(5) N7 0.124(7) 0.191(9) 0.128(6) -0.015(7) 0.034(5) 0.022(7) C42 0.114(8) 0.139(9) 0.203(12) 0.004(9) 0.038(8) 0.017(7) C43 0.177(13) 0.154(11) 0.67(4) 0.211(18) 0.087(18) 0.049(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 Ag1 N6 2.350(4) . ? Ag1 P1 2.4370(12) . ? Ag1 P2 2.4479(13) . ? P1 C1 1.805(5) . ? P1 C7 1.815(5) . ? P1 C13 1.853(5) . ? C1 C6 1.366(8) . ? C1 C2 1.392(7) . ? C2 C3 1.355(9) . ? C3 C4 1.339(10) . ? C4 C5 1.378(10) . ? C5 C6 1.391(8) . ? C7 C8 1.380(7) . ? C7 C12 1.392(7) . ? C8 C9 1.379(8) . ? C9 C10 1.361(10) . ? C10 C11 1.356(10) . ? C11 C12 1.386(9) . ? C13 N1 1.448(6) . ? N1 C14 1.355(6) . ? N2 C14 1.335(6) . ? N2 C18 1.341(6) . ? C14 C15 1.390(7) . ? C15 C16 1.379(7) . ? C16 C17 1.366(8) . ? C17 C18 1.352(8) . ? P2 C19 1.819(5) . ? P2 C25 1.823(5) . ? P2 C31 1.856(5) . ? C19 C24 1.375(7) . ? C19 C20 1.377(7) . ? C20 C21 1.368(8) . ? C21 C22 1.366(11) . ? C22 C23 1.374(10) . ? C23 C24 1.396(8) . ? C25 C26 1.347(7) . ? C25 C30 1.365(7) . ? C26 C27 1.392(7) . ? C27 C28 1.327(8) . ? C28 C29 1.357(9) . ? C29 C30 1.396(8) . ? C31 N3 1.427(7) . ? N3 C32 1.364(6) . ? N4 C32 1.323(6) . ? N4 C36 1.345(6) . ? C32 C33 1.397(7) . ? C33 C34 1.362(9) . ? C34 C35 1.381(9) . ? C35 C36 1.358(8) . ? N5 C37 1.189(9) . ? N5' C41 1.152(11) . ? N6 C37 1.353(7) . ? N6 C41 1.356(8) . ? C37 C38 1.402(10) . ? C38 C39 1.377(16) . ? C39 C40 1.342(16) . ? C40 C41 1.373(11) . ? Cl1 O4 1.362(6) . ? Cl1 O3 1.370(6) . ? Cl1 O2 1.392(6) . ? Cl1 O1 1.408(6) . ? N7 C42 1.183(12) . ? C42 C43 1.324(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ag1 P1 119.12(11) . . ? N6 Ag1 P2 112.88(11) . . ? P1 Ag1 P2 127.99(5) . . ? C1 P1 C7 103.7(2) . . ? C1 P1 C13 105.0(2) . . ? C7 P1 C13 101.8(2) . . ? C1 P1 Ag1 115.55(16) . . ? C7 P1 Ag1 119.93(17) . . ? C13 P1 Ag1 109.11(15) . . ? C6 C1 C2 117.6(5) . . ? C6 C1 P1 117.9(4) . . ? C2 C1 P1 124.5(4) . . ? C3 C2 C1 120.7(6) . . ? C4 C3 C2 121.8(7) . . ? C3 C4 C5 119.5(7) . . ? C4 C5 C6 119.3(7) . . ? C1 C6 C5 121.2(6) . . ? C8 C7 C12 118.2(5) . . ? C8 C7 P1 118.9(4) . . ? C12 C7 P1 122.9(4) . . ? C9 C8 C7 121.2(6) . . ? C10 C9 C8 120.2(7) . . ? C11 C10 C9 119.4(6) . . ? C10 C11 C12 121.8(7) . . ? C11 C12 C7 119.2(7) . . ? N1 C13 P1 112.1(3) . . ? C14 N1 C13 123.4(4) . . ? C14 N2 C18 116.5(4) . . ? N2 C14 N1 117.4(4) . . ? N2 C14 C15 122.8(4) . . ? N1 C14 C15 119.8(5) . . ? C16 C15 C14 117.7(5) . . ? C17 C16 C15 120.4(5) . . ? C18 C17 C16 117.3(5) . . ? N2 C18 C17 125.2(5) . . ? C19 P2 C25 103.6(2) . . ? C19 P2 C31 102.7(3) . . ? C25 P2 C31 102.6(2) . . ? C19 P2 Ag1 117.61(16) . . ? C25 P2 Ag1 118.14(17) . . ? C31 P2 Ag1 110.17(16) . . ? C24 C19 C20 118.4(5) . . ? C24 C19 P2 121.9(4) . . ? C20 C19 P2 119.7(4) . . ? C21 C20 C19 121.5(6) . . ? C22 C21 C20 119.9(7) . . ? C21 C22 C23 120.3(6) . . ? C22 C23 C24 119.2(7) . . ? C19 C24 C23 120.7(6) . . ? C26 C25 C30 117.8(5) . . ? C26 C25 P2 121.7(4) . . ? C30 C25 P2 120.2(4) . . ? C25 C26 C27 121.3(5) . . ? C28 C27 C26 120.6(6) . . ? C27 C28 C29 119.4(6) . . ? C28 C29 C30 120.0(6) . . ? C25 C30 C29 120.5(6) . . ? N3 C31 P2 113.2(3) . . ? C32 N3 C31 125.4(4) . . ? C32 N4 C36 117.5(5) . . ? N4 C32 N3 117.3(5) . . ? N4 C32 C33 122.8(5) . . ? N3 C32 C33 119.8(5) . . ? C34 C33 C32 118.3(6) . . ? C33 C34 C35 119.3(6) . . ? C36 C35 C34 118.7(6) . . ? N4 C36 C35 123.3(6) . . ? C37 N6 C41 119.5(5) . . ? C37 N6 Ag1 119.9(4) . . ? C41 N6 Ag1 119.9(4) . . ? N5 C37 N6 122.4(7) . . ? N5 C37 C38 118.2(8) . . ? N6 C37 C38 119.3(8) . . ? C39 C38 C37 119.2(9) . . ? C40 C39 C38 121.1(10) . . ? C39 C40 C41 118.5(11) . . ? N5' C41 N6 124.5(8) . . ? N5' C41 C40 113.3(10) . . ? N6 C41 C40 122.2(8) . . ? O4 Cl1 O3 112.1(6) . . ? O4 Cl1 O2 111.1(5) . . ? O3 Cl1 O2 110.5(5) . . ? O4 Cl1 O1 109.0(4) . . ? O3 Cl1 O1 106.1(4) . . ? O2 Cl1 O1 107.8(5) . . ? N7 C42 C43 176.5(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.650 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.068 #=============================================END data_compd8 #compound8 _database_code_CSD 171818 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H27 Cl2 N2 P Pd' _chemical_formula_weight 551.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2189(15) _cell_length_b 20.438(3) _cell_length_c 12.9647(19) _cell_angle_alpha 90.00 _cell_angle_beta 105.782(13) _cell_angle_gamma 90.00 _cell_volume 2350.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type PSI-Scans _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5765 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4576 _reflns_number_gt 2855 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0344P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00108(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4576 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.51974(5) 0.678380(19) -0.09708(3) 0.02942(12) Uani 1 1 d . . . Cl1 Cl 0.59043(17) 0.61985(7) -0.23689(11) 0.0488(4) Uani 1 1 d . . . Cl2 Cl 0.42285(16) 0.76296(6) -0.21088(10) 0.0431(4) Uani 1 1 d . . . P1 P 0.42238(15) 0.73142(6) 0.01506(10) 0.0275(3) Uani 1 1 d . . . N1 N 0.6203(5) 0.60812(19) 0.0191(3) 0.0311(10) Uani 1 1 d . . . N2 N 0.4565(5) 0.61687(19) 0.1289(3) 0.0317(10) Uani 1 1 d . . . C1 C 0.2182(6) 0.7307(2) -0.0201(4) 0.0309(12) Uani 1 1 d . . . C2 C 0.1354(6) 0.6983(2) -0.1121(4) 0.0354(13) Uani 1 1 d . . . H2A H 0.1850 0.6779 -0.1570 0.043 Uiso 1 1 calc R . . C3 C -0.0197(6) 0.6966(3) -0.1366(5) 0.0469(15) Uani 1 1 d . . . H3A H -0.0745 0.6739 -0.1967 0.056 Uiso 1 1 calc R . . C4 C -0.0939(7) 0.7286(3) -0.0719(5) 0.0517(16) Uani 1 1 d . . . H4A H -0.1987 0.7287 -0.0900 0.062 Uiso 1 1 calc R . . C5 C -0.0135(7) 0.7600(3) 0.0189(5) 0.0480(15) Uani 1 1 d . . . H5A H -0.0637 0.7811 0.0627 0.058 Uiso 1 1 calc R . . C6 C 0.1418(6) 0.7605(2) 0.0454(4) 0.0361(13) Uani 1 1 d . . . H6A H 0.1958 0.7811 0.1081 0.043 Uiso 1 1 calc R . . C7 C 0.4819(5) 0.8147(2) 0.0496(4) 0.0272(11) Uani 1 1 d . . . C8 C 0.3823(7) 0.8664(2) 0.0245(5) 0.0469(15) Uani 1 1 d . . . H8A H 0.2839 0.8593 -0.0165 0.056 Uiso 1 1 calc R . . C9 C 0.4281(8) 0.9287(3) 0.0601(5) 0.0586(19) Uani 1 1 d . . . H9A H 0.3595 0.9631 0.0445 0.070 Uiso 1 1 calc R . . C10 C 0.5732(8) 0.9401(3) 0.1179(5) 0.0530(17) Uani 1 1 d . . . H10A H 0.6025 0.9820 0.1432 0.064 Uiso 1 1 calc R . . C11 C 0.6757(7) 0.8902(3) 0.1388(4) 0.0490(16) Uani 1 1 d . . . H11A H 0.7757 0.8984 0.1753 0.059 Uiso 1 1 calc R . . C12 C 0.6295(6) 0.8266(3) 0.1049(4) 0.0357(12) Uani 1 1 d . . . H12A H 0.6987 0.7925 0.1197 0.043 Uiso 1 1 calc R . . C13 C 0.4831(6) 0.6877(2) 0.1424(4) 0.0311(12) Uani 1 1 d . . . H13A H 0.5898 0.6955 0.1741 0.037 Uiso 1 1 calc R . . H13B H 0.4289 0.7046 0.1912 0.037 Uiso 1 1 calc R . . C14 C 0.5595(6) 0.5810(2) 0.0941(4) 0.0316(12) Uani 1 1 d . . . C15 C 0.6062(6) 0.5181(2) 0.1343(4) 0.0390(14) Uani 1 1 d . . . H15A H 0.5592 0.4978 0.1807 0.047 Uiso 1 1 calc R . . C16 C 0.7184(7) 0.4875(3) 0.1060(4) 0.0470(16) Uani 1 1 d . . . H16A H 0.7462 0.4454 0.1307 0.056 Uiso 1 1 calc R . . C17 C 0.7929(7) 0.5184(3) 0.0399(5) 0.0476(15) Uani 1 1 d . . . H17A H 0.8768 0.4994 0.0252 0.057 Uiso 1 1 calc R . . C18 C 0.7390(6) 0.5774(3) -0.0026(4) 0.0418(14) Uani 1 1 d . . . H18A H 0.7861 0.5977 -0.0490 0.050 Uiso 1 1 calc R . . C19 C 0.3747(6) 0.5869(2) 0.2009(4) 0.0375(13) Uani 1 1 d . . . H19A H 0.3656 0.5400 0.1842 0.045 Uiso 1 1 calc R . . C20 C 0.4626(7) 0.5931(3) 0.3186(4) 0.0479(16) Uani 1 1 d . . . H20A H 0.4808 0.6389 0.3367 0.057 Uiso 1 1 calc R . . H20B H 0.5594 0.5715 0.3301 0.057 Uiso 1 1 calc R . . C21 C 0.3751(8) 0.5621(3) 0.3923(5) 0.062(2) Uani 1 1 d . . . H21A H 0.3701 0.5150 0.3818 0.074 Uiso 1 1 calc R . . H21B H 0.4282 0.5706 0.4665 0.074 Uiso 1 1 calc R . . C22 C 0.2158(8) 0.5897(3) 0.3683(5) 0.065(2) Uani 1 1 d . . . H22A H 0.1619 0.5681 0.4133 0.078 Uiso 1 1 calc R . . H22B H 0.2210 0.6360 0.3854 0.078 Uiso 1 1 calc R . . C23 C 0.1310(7) 0.5805(3) 0.2525(5) 0.0559(18) Uani 1 1 d . . . H23A H 0.0310 0.5992 0.2393 0.067 Uiso 1 1 calc R . . H23B H 0.1203 0.5341 0.2360 0.067 Uiso 1 1 calc R . . C24 C 0.2156(6) 0.6135(3) 0.1810(4) 0.0456(15) Uani 1 1 d . . . H24A H 0.1612 0.6066 0.1065 0.055 Uiso 1 1 calc R . . H24B H 0.2201 0.6602 0.1946 0.055 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 0.0321(2) 0.02726(19) 0.0300(2) -0.0002(2) 0.01031(16) -0.0017(2) Cl1 0.0546(10) 0.0510(9) 0.0461(8) -0.0089(7) 0.0229(8) 0.0005(8) Cl2 0.0512(9) 0.0401(8) 0.0359(7) 0.0081(6) 0.0084(7) -0.0036(7) P1 0.0295(8) 0.0249(7) 0.0273(7) 0.0005(6) 0.0065(6) 0.0011(6) N1 0.031(3) 0.028(2) 0.037(2) 0.001(2) 0.013(2) 0.006(2) N2 0.043(3) 0.025(2) 0.028(2) 0.0001(18) 0.011(2) -0.002(2) C1 0.030(3) 0.029(3) 0.032(3) 0.006(2) 0.006(2) 0.004(2) C2 0.041(3) 0.034(3) 0.030(3) 0.002(2) 0.007(3) -0.003(3) C3 0.039(4) 0.047(4) 0.046(3) 0.000(3) -0.001(3) -0.015(3) C4 0.030(3) 0.051(4) 0.071(4) 0.014(3) 0.010(3) -0.007(3) C5 0.045(4) 0.045(3) 0.063(4) 0.010(3) 0.029(3) 0.007(3) C6 0.035(3) 0.039(3) 0.035(3) -0.001(2) 0.011(3) 0.005(3) C7 0.033(3) 0.021(2) 0.028(2) 0.001(2) 0.008(2) -0.006(2) C8 0.043(4) 0.030(3) 0.060(4) 0.003(3) 0.000(3) 0.001(3) C9 0.062(5) 0.031(3) 0.086(5) 0.002(3) 0.024(4) 0.007(3) C10 0.077(5) 0.032(3) 0.052(4) -0.006(3) 0.021(4) -0.013(4) C11 0.056(4) 0.050(4) 0.034(3) 0.002(3) 0.000(3) -0.021(3) C12 0.036(3) 0.037(3) 0.031(3) 0.006(3) 0.003(2) -0.001(3) C13 0.035(3) 0.026(3) 0.031(2) -0.006(2) 0.007(2) -0.005(3) C14 0.037(3) 0.026(3) 0.028(3) -0.001(2) 0.002(2) -0.001(3) C15 0.052(4) 0.028(3) 0.037(3) 0.007(2) 0.012(3) 0.006(3) C16 0.057(4) 0.028(3) 0.051(4) 0.004(3) 0.006(3) 0.014(3) C17 0.039(4) 0.042(4) 0.060(4) -0.006(3) 0.011(3) 0.016(3) C18 0.037(3) 0.045(3) 0.045(3) 0.004(3) 0.015(3) 0.002(3) C19 0.051(4) 0.028(3) 0.036(3) 0.001(2) 0.016(3) -0.001(3) C20 0.069(4) 0.038(3) 0.035(3) 0.000(3) 0.013(3) 0.001(3) C21 0.112(6) 0.037(3) 0.042(4) 0.010(3) 0.029(4) -0.003(4) C22 0.113(6) 0.035(3) 0.069(5) -0.002(3) 0.061(5) -0.010(4) C23 0.070(5) 0.039(3) 0.073(5) -0.004(3) 0.042(4) -0.005(3) C24 0.055(4) 0.037(3) 0.050(4) 0.004(3) 0.024(3) -0.003(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 2.105(4) . ? Pd1 P1 2.1918(14) . ? Pd1 Cl2 2.2904(14) . ? Pd1 Cl1 2.4050(14) . ? P1 C7 1.806(5) . ? P1 C1 1.812(5) . ? P1 C13 1.826(5) . ? N1 C18 1.356(6) . ? N1 C14 1.366(6) . ? N2 C14 1.370(6) . ? N2 C13 1.471(5) . ? N2 C19 1.483(6) . ? C1 C6 1.384(6) . ? C1 C2 1.396(7) . ? C2 C3 1.379(7) . ? C3 C4 1.383(8) . ? C4 C5 1.368(8) . ? C5 C6 1.378(7) . ? C7 C12 1.376(6) . ? C7 C8 1.381(7) . ? C8 C9 1.380(7) . ? C9 C10 1.364(8) . ? C10 C11 1.366(8) . ? C11 C12 1.400(7) . ? C14 C15 1.409(7) . ? C15 C16 1.342(7) . ? C16 C17 1.387(7) . ? C17 C18 1.363(7) . ? C19 C24 1.519(7) . ? C19 C20 1.526(7) . ? C20 C21 1.543(7) . ? C21 C22 1.524(8) . ? C22 C23 1.505(8) . ? C23 C24 1.521(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 P1 92.46(11) . . ? N1 Pd1 Cl2 174.00(12) . . ? P1 Pd1 Cl2 84.02(5) . . ? N1 Pd1 Cl1 92.47(11) . . ? P1 Pd1 Cl1 171.78(6) . . ? Cl2 Pd1 Cl1 91.60(5) . . ? C7 P1 C1 107.1(2) . . ? C7 P1 C13 103.8(2) . . ? C1 P1 C13 105.4(2) . . ? C7 P1 Pd1 118.59(16) . . ? C1 P1 Pd1 114.45(17) . . ? C13 P1 Pd1 106.11(16) . . ? C18 N1 C14 118.1(4) . . ? C18 N1 Pd1 113.0(3) . . ? C14 N1 Pd1 126.9(3) . . ? C14 N2 C13 117.2(4) . . ? C14 N2 C19 120.2(4) . . ? C13 N2 C19 115.4(4) . . ? C6 C1 C2 118.8(5) . . ? C6 C1 P1 120.6(4) . . ? C2 C1 P1 120.5(4) . . ? C3 C2 C1 120.0(5) . . ? C2 C3 C4 120.2(5) . . ? C5 C4 C3 120.1(6) . . ? C4 C5 C6 120.1(6) . . ? C5 C6 C1 120.7(5) . . ? C12 C7 C8 119.1(5) . . ? C12 C7 P1 119.2(4) . . ? C8 C7 P1 121.7(4) . . ? C9 C8 C7 120.3(5) . . ? C10 C9 C8 120.4(6) . . ? C9 C10 C11 120.2(6) . . ? C10 C11 C12 119.7(6) . . ? C7 C12 C11 120.1(5) . . ? N2 C13 P1 112.0(3) . . ? N1 C14 N2 118.2(4) . . ? N1 C14 C15 119.4(5) . . ? N2 C14 C15 122.4(5) . . ? C16 C15 C14 120.3(5) . . ? C15 C16 C17 120.3(5) . . ? C18 C17 C16 117.7(5) . . ? N1 C18 C17 123.5(5) . . ? N2 C19 C24 112.2(4) . . ? N2 C19 C20 111.9(5) . . ? C24 C19 C20 111.4(5) . . ? C19 C20 C21 111.1(5) . . ? C22 C21 C20 111.0(5) . . ? C23 C22 C21 111.5(5) . . ? C22 C23 C24 109.8(5) . . ? C19 C24 C23 111.6(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.425 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.099 #=================================================END data_compd9 #compound9 _database_code_CSD 171819 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H54 Cl Cu N4 O4 P2' _chemical_formula_weight 911.88 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0567(8) _cell_length_b 11.0961(6) _cell_length_c 26.8423(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.7230(10) _cell_angle_gamma 90.00 _cell_volume 4484.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.532186 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29874 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10772 _reflns_number_gt 6253 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0644P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10772 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.21597(2) 0.04532(3) 0.107376(11) 0.04053(11) Uani 1 1 d . . . P1 P 0.24663(5) 0.20841(6) 0.06234(2) 0.03816(17) Uani 1 1 d . . . P2 P 0.25321(5) -0.01248(6) 0.18355(2) 0.03621(17) Uani 1 1 d . . . N1 N 0.20748(16) -0.0721(2) 0.04582(8) 0.0445(6) Uani 1 1 d . . . N2 N 0.29521(15) 0.0406(2) -0.00818(8) 0.0443(5) Uani 1 1 d . . . N3 N 0.07489(14) 0.0627(2) 0.12338(8) 0.0439(6) Uani 1 1 d . . . N4 N 0.10322(14) 0.1347(2) 0.20366(7) 0.0395(5) Uani 1 1 d . . . C1 C 0.15830(18) 0.3195(2) 0.06886(11) 0.0445(7) Uani 1 1 d . . . C2 C 0.0874(2) 0.3336(3) 0.03718(14) 0.0667(9) Uani 1 1 d . . . H2A H 0.0859 0.2937 0.0067 0.080 Uiso 1 1 calc R . . C3 C 0.0162(2) 0.4096(4) 0.05100(18) 0.0833(12) Uani 1 1 d . . . H3A H -0.0333 0.4170 0.0302 0.100 Uiso 1 1 calc R . . C4 C 0.0202(3) 0.4714(4) 0.09445(18) 0.0825(12) Uani 1 1 d . . . H4A H -0.0266 0.5218 0.1030 0.099 Uiso 1 1 calc R . . C5 C 0.0914(3) 0.4608(3) 0.12566(16) 0.0793(11) Uani 1 1 d . . . H5A H 0.0943 0.5053 0.1550 0.095 Uiso 1 1 calc R . . C6 C 0.1592(2) 0.3838(3) 0.11351(12) 0.0631(9) Uani 1 1 d . . . H6A H 0.2068 0.3743 0.1356 0.076 Uiso 1 1 calc R . . C7 C 0.34604(18) 0.3014(2) 0.06407(10) 0.0422(6) Uani 1 1 d . . . C8 C 0.3460(2) 0.4163(3) 0.04349(12) 0.0580(8) Uani 1 1 d . . . H8A H 0.2957 0.4447 0.0268 0.070 Uiso 1 1 calc R . . C9 C 0.4207(3) 0.4886(3) 0.04770(16) 0.0783(11) Uani 1 1 d . . . H9A H 0.4203 0.5655 0.0339 0.094 Uiso 1 1 calc R . . C10 C 0.4955(3) 0.4470(4) 0.07222(16) 0.0824(12) Uani 1 1 d . . . H10A H 0.5453 0.4961 0.0753 0.099 Uiso 1 1 calc R . . C11 C 0.4966(2) 0.3337(4) 0.09204(13) 0.0740(10) Uani 1 1 d . . . H11A H 0.5473 0.3055 0.1083 0.089 Uiso 1 1 calc R . . C12 C 0.42199(19) 0.2604(3) 0.08790(11) 0.0557(8) Uani 1 1 d . . . H12A H 0.4233 0.1831 0.1013 0.067 Uiso 1 1 calc R . . C13 C 0.23863(18) 0.1469(2) -0.00185(9) 0.0436(7) Uani 1 1 d . . . H13A H 0.1774 0.1253 -0.0092 0.052 Uiso 1 1 calc R . . H13B H 0.2561 0.2086 -0.0254 0.052 Uiso 1 1 calc R . . C14 C 0.26304(18) -0.0703(2) 0.00656(9) 0.0417(6) Uani 1 1 d . . . C15 C 0.2845(2) -0.1785(3) -0.01752(11) 0.0570(8) Uani 1 1 d . . . H15A H 0.3240 -0.1777 -0.0439 0.068 Uiso 1 1 calc R . . C16 C 0.2477(3) -0.2852(3) -0.00263(12) 0.0675(10) Uani 1 1 d . . . H16A H 0.2624 -0.3567 -0.0186 0.081 Uiso 1 1 calc R . . C17 C 0.1888(3) -0.2859(3) 0.03616(12) 0.0673(10) Uani 1 1 d . . . H17A H 0.1619 -0.3569 0.0465 0.081 Uiso 1 1 calc R . . C18 C 0.1716(2) -0.1794(3) 0.05865(11) 0.0571(8) Uani 1 1 d . . . H18A H 0.1320 -0.1800 0.0850 0.068 Uiso 1 1 calc R . . C19 C 0.36564(19) 0.0451(3) -0.04594(10) 0.0496(7) Uani 1 1 d . . . H19A H 0.3992 -0.0302 -0.0425 0.060 Uiso 1 1 calc R . . C20 C 0.3296(2) 0.0473(3) -0.09913(11) 0.0627(9) Uani 1 1 d . . . H20A H 0.2966 0.1213 -0.1047 0.075 Uiso 1 1 calc R . . H20B H 0.2892 -0.0199 -0.1041 0.075 Uiso 1 1 calc R . . C21 C 0.4049(3) 0.0391(4) -0.13637(13) 0.0852(12) Uani 1 1 d . . . H21A H 0.4327 -0.0396 -0.1337 0.102 Uiso 1 1 calc R . . H21B H 0.3808 0.0472 -0.1699 0.102 Uiso 1 1 calc R . . C22 C 0.4738(3) 0.1348(4) -0.12763(13) 0.0877(13) Uani 1 1 d . . . H22A H 0.4483 0.2130 -0.1353 0.105 Uiso 1 1 calc R . . H22B H 0.5231 0.1216 -0.1499 0.105 Uiso 1 1 calc R . . C23 C 0.5081(2) 0.1347(4) -0.07405(13) 0.0784(11) Uani 1 1 d . . . H23A H 0.5491 0.2013 -0.0693 0.094 Uiso 1 1 calc R . . H23B H 0.5401 0.0604 -0.0675 0.094 Uiso 1 1 calc R . . C24 C 0.4319(2) 0.1464(3) -0.03745(12) 0.0651(9) Uani 1 1 d . . . H24A H 0.4550 0.1429 -0.0036 0.078 Uiso 1 1 calc R . . H24B H 0.4026 0.2235 -0.0421 0.078 Uiso 1 1 calc R . . C25 C 0.26634(17) -0.1716(2) 0.20005(10) 0.0413(6) Uani 1 1 d . . . C26 C 0.29441(18) -0.2505(3) 0.16364(11) 0.0503(7) Uani 1 1 d . . . H26A H 0.3074 -0.2215 0.1320 0.060 Uiso 1 1 calc R . . C27 C 0.3033(2) -0.3724(3) 0.17380(14) 0.0659(9) Uani 1 1 d . . . H27A H 0.3228 -0.4249 0.1492 0.079 Uiso 1 1 calc R . . C28 C 0.2832(2) -0.4157(3) 0.22045(16) 0.0730(10) Uani 1 1 d . . . H28A H 0.2886 -0.4976 0.2272 0.088 Uiso 1 1 calc R . . C29 C 0.2550(2) -0.3385(3) 0.25696(14) 0.0702(10) Uani 1 1 d . . . H29A H 0.2418 -0.3680 0.2884 0.084 Uiso 1 1 calc R . . C30 C 0.24654(19) -0.2174(3) 0.24688(11) 0.0543(8) Uani 1 1 d . . . H30A H 0.2273 -0.1654 0.2717 0.065 Uiso 1 1 calc R . . C31 C 0.34423(17) 0.0644(2) 0.21627(10) 0.0414(6) Uani 1 1 d . . . C32 C 0.3947(2) 0.0139(3) 0.25370(13) 0.0662(10) Uani 1 1 d . . . H32A H 0.3823 -0.0639 0.2645 0.079 Uiso 1 1 calc R . . C33 C 0.4637(2) 0.0777(4) 0.27542(15) 0.0827(12) Uani 1 1 d . . . H33A H 0.4968 0.0427 0.3010 0.099 Uiso 1 1 calc R . . C34 C 0.4840(2) 0.1915(4) 0.25990(13) 0.0684(10) Uani 1 1 d . . . H34A H 0.5321 0.2326 0.2738 0.082 Uiso 1 1 calc R . . C35 C 0.4329(3) 0.2433(3) 0.22403(14) 0.0762(11) Uani 1 1 d . . . H35A H 0.4447 0.3219 0.2141 0.091 Uiso 1 1 calc R . . C36 C 0.3630(2) 0.1805(3) 0.20189(12) 0.0614(9) Uani 1 1 d . . . H36A H 0.3287 0.2172 0.1772 0.074 Uiso 1 1 calc R . . C37 C 0.15102(17) 0.0248(2) 0.21859(10) 0.0396(6) Uani 1 1 d . . . H37A H 0.1103 -0.0427 0.2155 0.047 Uiso 1 1 calc R . . H37B H 0.1671 0.0320 0.2536 0.047 Uiso 1 1 calc R . . C38 C 0.04726(17) 0.1290(2) 0.16232(10) 0.0406(6) Uani 1 1 d . . . C39 C -0.03484(19) 0.1886(3) 0.15992(11) 0.0555(8) Uani 1 1 d . . . H39A H -0.0537 0.2345 0.1868 0.067 Uiso 1 1 calc R . . C40 C -0.0872(2) 0.1792(3) 0.11797(13) 0.0648(9) Uani 1 1 d . . . H40A H -0.1410 0.2202 0.1159 0.078 Uiso 1 1 calc R . . C41 C -0.0600(2) 0.1092(3) 0.07914(12) 0.0602(9) Uani 1 1 d . . . H41A H -0.0954 0.0998 0.0508 0.072 Uiso 1 1 calc R . . C42 C 0.0205(2) 0.0538(3) 0.08326(11) 0.0538(8) Uani 1 1 d . . . H42A H 0.0391 0.0068 0.0567 0.065 Uiso 1 1 calc R . . C43 C 0.08407(18) 0.2200(2) 0.24438(10) 0.0443(7) Uani 1 1 d . . . H43A H 0.0514 0.2874 0.2294 0.053 Uiso 1 1 calc R . . C44 C 0.0244(2) 0.1669(3) 0.28429(11) 0.0555(8) Uani 1 1 d . . . H44A H -0.0319 0.1435 0.2693 0.067 Uiso 1 1 calc R . . H44B H 0.0522 0.0952 0.2981 0.067 Uiso 1 1 calc R . . C45 C 0.0078(3) 0.2567(4) 0.32600(14) 0.0866(13) Uani 1 1 d . . . H45A H -0.0241 0.2170 0.3525 0.104 Uiso 1 1 calc R . . H45B H -0.0291 0.3218 0.3134 0.104 Uiso 1 1 calc R . . C46 C 0.0942(3) 0.3087(4) 0.34695(14) 0.0892(13) Uani 1 1 d . . . H46A H 0.0809 0.3693 0.3718 0.107 Uiso 1 1 calc R . . H46B H 0.1283 0.2452 0.3630 0.107 Uiso 1 1 calc R . . C47 C 0.1481(3) 0.3645(3) 0.30620(13) 0.0808(11) Uani 1 1 d . . . H47A H 0.2031 0.3961 0.3202 0.097 Uiso 1 1 calc R . . H47B H 0.1154 0.4309 0.2914 0.097 Uiso 1 1 calc R . . C48 C 0.1690(2) 0.2719(3) 0.26634(11) 0.0579(8) Uani 1 1 d . . . H48A H 0.2031 0.3096 0.2402 0.069 Uiso 1 1 calc R . . H48B H 0.2046 0.2076 0.2807 0.069 Uiso 1 1 calc R . . Cl1 Cl 0.24822(6) 0.00789(9) 0.38246(3) 0.0711(3) Uani 1 1 d . . . O1 O 0.1840(2) -0.0040(3) 0.34453(11) 0.1106(11) Uani 1 1 d . . . O2 O 0.2941(2) -0.1033(3) 0.38683(12) 0.1184(11) Uani 1 1 d . . . O3 O 0.2048(2) 0.0340(3) 0.42706(11) 0.1174(11) Uani 1 1 d . . . O4 O 0.3072(3) 0.1006(4) 0.37122(19) 0.1774(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0456(2) 0.0435(2) 0.03241(17) 0.00239(14) -0.00262(14) -0.00845(15) P1 0.0397(4) 0.0372(4) 0.0376(4) 0.0016(3) 0.0002(3) -0.0026(3) P2 0.0364(4) 0.0382(4) 0.0339(3) 0.0011(3) -0.0033(3) -0.0029(3) N1 0.0552(15) 0.0429(14) 0.0354(12) -0.0025(10) -0.0024(11) -0.0132(11) N2 0.0510(14) 0.0454(14) 0.0366(12) 0.0008(10) 0.0058(10) -0.0008(11) N3 0.0367(13) 0.0523(15) 0.0423(12) 0.0047(11) -0.0071(10) -0.0074(10) N4 0.0370(12) 0.0422(13) 0.0391(12) 0.0026(10) -0.0062(10) 0.0047(10) C1 0.0373(15) 0.0394(16) 0.0569(17) 0.0086(13) 0.0057(13) -0.0017(12) C2 0.055(2) 0.059(2) 0.086(2) -0.0006(18) -0.0103(19) 0.0028(17) C3 0.052(2) 0.074(3) 0.123(4) 0.014(3) -0.018(2) -0.0013(19) C4 0.062(3) 0.064(3) 0.122(4) -0.001(2) 0.022(3) 0.0042(19) C5 0.079(3) 0.073(3) 0.086(3) -0.004(2) 0.023(2) 0.013(2) C6 0.067(2) 0.059(2) 0.064(2) -0.0032(17) 0.0086(17) 0.0127(17) C7 0.0406(15) 0.0423(16) 0.0438(14) -0.0009(12) 0.0050(12) -0.0041(12) C8 0.0512(19) 0.0529(19) 0.070(2) 0.0080(16) 0.0018(16) -0.0091(15) C9 0.072(3) 0.058(2) 0.105(3) 0.010(2) 0.012(2) -0.0204(19) C10 0.061(2) 0.090(3) 0.097(3) -0.006(2) 0.005(2) -0.034(2) C11 0.0432(19) 0.101(3) 0.078(2) 0.002(2) -0.0095(17) -0.0134(19) C12 0.0471(18) 0.059(2) 0.0606(19) 0.0008(16) -0.0031(15) -0.0027(15) C13 0.0475(16) 0.0459(17) 0.0372(14) 0.0079(12) -0.0010(12) -0.0033(13) C14 0.0453(16) 0.0446(17) 0.0350(14) -0.0035(12) -0.0084(12) -0.0007(12) C15 0.068(2) 0.057(2) 0.0461(17) -0.0067(15) -0.0010(15) 0.0088(16) C16 0.099(3) 0.0422(19) 0.061(2) -0.0069(16) -0.013(2) 0.0039(18) C17 0.099(3) 0.046(2) 0.057(2) 0.0026(16) -0.017(2) -0.0203(18) C18 0.074(2) 0.0509(19) 0.0460(16) 0.0003(15) -0.0026(15) -0.0187(16) C19 0.0467(17) 0.062(2) 0.0401(15) -0.0008(14) 0.0056(13) -0.0024(15) C20 0.058(2) 0.089(3) 0.0414(16) -0.0016(16) 0.0018(15) -0.0023(18) C21 0.081(3) 0.132(4) 0.0420(19) -0.007(2) 0.0100(18) 0.001(3) C22 0.080(3) 0.122(4) 0.062(2) 0.015(2) 0.027(2) -0.001(3) C23 0.060(2) 0.104(3) 0.071(2) -0.005(2) 0.0203(18) -0.015(2) C24 0.059(2) 0.083(3) 0.0535(18) -0.0030(17) 0.0093(16) -0.0094(18) C25 0.0371(15) 0.0423(16) 0.0445(15) 0.0013(12) -0.0048(12) -0.0007(12) C26 0.0482(17) 0.0500(18) 0.0525(17) -0.0080(14) -0.0067(14) -0.0021(14) C27 0.063(2) 0.049(2) 0.086(3) -0.0172(19) -0.0094(19) 0.0029(16) C28 0.064(2) 0.045(2) 0.109(3) 0.009(2) -0.006(2) -0.0020(17) C29 0.070(2) 0.059(2) 0.082(2) 0.028(2) 0.011(2) 0.0043(18) C30 0.0553(19) 0.0508(19) 0.0569(18) 0.0081(15) 0.0066(15) 0.0070(14) C31 0.0357(14) 0.0492(18) 0.0393(14) -0.0049(12) -0.0006(12) -0.0026(12) C32 0.061(2) 0.056(2) 0.080(2) 0.0043(17) -0.0300(19) -0.0058(16) C33 0.069(2) 0.084(3) 0.094(3) -0.002(2) -0.044(2) -0.004(2) C34 0.050(2) 0.082(3) 0.072(2) -0.020(2) -0.0140(17) -0.0134(18) C35 0.081(3) 0.069(2) 0.079(2) 0.001(2) -0.012(2) -0.031(2) C36 0.062(2) 0.063(2) 0.0587(19) 0.0101(16) -0.0157(16) -0.0183(17) C37 0.0387(15) 0.0422(16) 0.0377(14) 0.0028(12) -0.0045(11) -0.0010(12) C38 0.0376(15) 0.0399(16) 0.0444(15) 0.0116(13) -0.0036(12) -0.0069(12) C39 0.0440(17) 0.067(2) 0.0554(18) 0.0070(15) -0.0059(15) 0.0047(15) C40 0.0403(18) 0.075(2) 0.078(2) 0.019(2) -0.0151(17) 0.0025(16) C41 0.0442(18) 0.080(2) 0.0561(19) 0.0177(18) -0.0195(15) -0.0122(16) C42 0.0459(18) 0.070(2) 0.0451(16) 0.0046(15) -0.0119(14) -0.0151(15) C43 0.0476(17) 0.0398(16) 0.0453(15) 0.0044(12) -0.0049(13) 0.0078(13) C44 0.0567(19) 0.0546(19) 0.0555(18) 0.0040(15) 0.0046(15) 0.0139(15) C45 0.107(3) 0.080(3) 0.074(2) 0.006(2) 0.027(2) 0.051(2) C46 0.133(4) 0.074(3) 0.061(2) -0.028(2) -0.007(2) 0.036(3) C47 0.117(3) 0.055(2) 0.071(2) -0.0112(19) -0.023(2) 0.003(2) C48 0.069(2) 0.0494(19) 0.0555(18) -0.0032(15) -0.0075(16) -0.0098(16) Cl1 0.0517(5) 0.0972(7) 0.0644(5) 0.0260(5) -0.0001(4) 0.0095(5) O1 0.104(2) 0.149(3) 0.0776(19) -0.0021(18) -0.0304(17) 0.044(2) O2 0.094(2) 0.140(3) 0.120(2) 0.033(2) -0.0016(19) 0.057(2) O3 0.132(3) 0.154(3) 0.0666(18) -0.0009(18) 0.0034(18) 0.027(2) O4 0.125(3) 0.161(4) 0.247(5) 0.060(4) 0.039(3) -0.048(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 Cu1 N1 2.107(2) . ? Cu1 N3 2.181(2) . ? Cu1 P2 2.2086(7) . ? Cu1 P1 2.2279(7) . ? P1 C7 1.818(3) . ? P1 C1 1.823(3) . ? P1 C13 1.856(3) . ? P2 C31 1.829(3) . ? P2 C25 1.830(3) . ? P2 C37 1.860(3) . ? N1 C14 1.354(3) . ? N1 C18 1.354(3) . ? N2 C14 1.382(3) . ? N2 C13 1.466(3) . ? N2 C19 1.477(3) . ? N3 C42 1.348(3) . ? N3 C38 1.349(3) . ? N4 C38 1.386(3) . ? N4 C37 1.469(3) . ? N4 C43 1.477(3) . ? C1 C2 1.365(4) . ? C1 C6 1.395(4) . ? C2 C3 1.417(5) . ? C3 C4 1.354(5) . ? C4 C5 1.357(5) . ? C5 C6 1.374(5) . ? C7 C12 1.380(4) . ? C7 C8 1.389(4) . ? C8 C9 1.385(4) . ? C9 C10 1.377(5) . ? C10 C11 1.365(5) . ? C11 C12 1.390(4) . ? C14 C15 1.403(4) . ? C15 C16 1.369(4) . ? C16 C17 1.376(5) . ? C17 C18 1.353(4) . ? C19 C24 1.519(4) . ? C19 C20 1.521(4) . ? C20 C21 1.524(5) . ? C21 C22 1.501(5) . ? C22 C23 1.522(5) . ? C23 C24 1.525(4) . ? C25 C26 1.383(4) . ? C25 C30 1.392(4) . ? C26 C27 1.387(4) . ? C27 C28 1.378(5) . ? C28 C29 1.372(5) . ? C29 C30 1.377(4) . ? C31 C32 1.372(4) . ? C31 C36 1.375(4) . ? C32 C33 1.380(4) . ? C33 C34 1.365(5) . ? C34 C35 1.353(5) . ? C35 C36 1.390(4) . ? C38 C39 1.403(4) . ? C39 C40 1.371(4) . ? C40 C41 1.367(5) . ? C41 C42 1.363(4) . ? C43 C48 1.515(4) . ? C43 C44 1.525(4) . ? C44 C45 1.522(4) . ? C45 C46 1.524(6) . ? C46 C47 1.504(5) . ? C47 C48 1.518(4) . ? Cl1 O4 1.395(4) . ? Cl1 O1 1.401(3) . ? Cl1 O3 1.402(3) . ? Cl1 O2 1.418(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 99.18(9) . . ? N1 Cu1 P2 123.96(7) . . ? N3 Cu1 P2 94.58(6) . . ? N1 Cu1 P1 95.04(6) . . ? N3 Cu1 P1 104.13(6) . . ? P2 Cu1 P1 133.34(3) . . ? C7 P1 C1 102.44(13) . . ? C7 P1 C13 106.03(12) . . ? C1 P1 C13 107.39(13) . . ? C7 P1 Cu1 128.55(9) . . ? C1 P1 Cu1 109.91(9) . . ? C13 P1 Cu1 101.16(9) . . ? C31 P2 C25 104.82(12) . . ? C31 P2 C37 105.86(12) . . ? C25 P2 C37 100.34(12) . . ? C31 P2 Cu1 119.26(9) . . ? C25 P2 Cu1 121.97(9) . . ? C37 P2 Cu1 101.63(8) . . ? C14 N1 C18 117.6(2) . . ? C14 N1 Cu1 124.70(17) . . ? C18 N1 Cu1 111.41(18) . . ? C14 N2 C13 118.5(2) . . ? C14 N2 C19 118.9(2) . . ? C13 N2 C19 118.4(2) . . ? C42 N3 C38 118.0(2) . . ? C42 N3 Cu1 114.81(19) . . ? C38 N3 Cu1 120.77(17) . . ? C38 N4 C37 118.1(2) . . ? C38 N4 C43 119.9(2) . . ? C37 N4 C43 115.46(19) . . ? C2 C1 C6 118.4(3) . . ? C2 C1 P1 125.7(2) . . ? C6 C1 P1 115.4(2) . . ? C1 C2 C3 119.6(3) . . ? C4 C3 C2 120.1(4) . . ? C3 C4 C5 120.9(4) . . ? C4 C5 C6 119.4(4) . . ? C5 C6 C1 121.5(3) . . ? C12 C7 C8 118.9(3) . . ? C12 C7 P1 120.1(2) . . ? C8 C7 P1 121.0(2) . . ? C9 C8 C7 120.2(3) . . ? C10 C9 C8 120.2(4) . . ? C11 C10 C9 120.0(3) . . ? C10 C11 C12 120.2(3) . . ? C7 C12 C11 120.5(3) . . ? N2 C13 P1 111.86(17) . . ? N1 C14 N2 117.3(2) . . ? N1 C14 C15 119.6(3) . . ? N2 C14 C15 123.1(3) . . ? C16 C15 C14 120.6(3) . . ? C15 C16 C17 119.5(3) . . ? C18 C17 C16 117.5(3) . . ? C17 C18 N1 125.1(3) . . ? N2 C19 C24 113.4(2) . . ? N2 C19 C20 113.2(2) . . ? C24 C19 C20 110.8(3) . . ? C19 C20 C21 110.8(3) . . ? C22 C21 C20 112.0(3) . . ? C21 C22 C23 111.9(3) . . ? C22 C23 C24 111.1(3) . . ? C19 C24 C23 109.8(3) . . ? C26 C25 C30 118.6(3) . . ? C26 C25 P2 118.2(2) . . ? C30 C25 P2 123.2(2) . . ? C25 C26 C27 120.6(3) . . ? C28 C27 C26 119.8(3) . . ? C29 C28 C27 120.3(3) . . ? C28 C29 C30 119.8(3) . . ? C29 C30 C25 120.9(3) . . ? C32 C31 C36 118.3(3) . . ? C32 C31 P2 124.4(2) . . ? C36 C31 P2 117.2(2) . . ? C31 C32 C33 120.4(3) . . ? C34 C33 C32 121.0(3) . . ? C35 C34 C33 118.9(3) . . ? C34 C35 C36 120.7(3) . . ? C31 C36 C35 120.5(3) . . ? N4 C37 P2 116.88(18) . . ? N3 C38 N4 117.0(2) . . ? N3 C38 C39 120.1(2) . . ? N4 C38 C39 122.8(3) . . ? C40 C39 C38 120.0(3) . . ? C41 C40 C39 119.7(3) . . ? C42 C41 C40 118.0(3) . . ? N3 C42 C41 124.2(3) . . ? N4 C43 C48 111.1(2) . . ? N4 C43 C44 113.2(2) . . ? C48 C43 C44 112.0(2) . . ? C45 C44 C43 111.6(3) . . ? C44 C45 C46 111.8(3) . . ? C47 C46 C45 110.7(3) . . ? C46 C47 C48 110.7(3) . . ? C43 C48 C47 110.5(3) . . ? O4 Cl1 O1 110.3(3) . . ? O4 Cl1 O3 109.7(3) . . ? O1 Cl1 O3 108.4(2) . . ? O4 Cl1 O2 110.4(3) . . ? O1 Cl1 O2 108.0(2) . . ? O3 Cl1 O2 109.95(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.803 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.064 #================================================END data_compd10b #compound10b _database_code_CSD 171820 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C97 H110 Ag3 Cl5 N8 O12 P4' _chemical_formula_weight 2204.67 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 21.413(3) _cell_length_b 9.5311(15) _cell_length_c 26.950(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.207(4) _cell_angle_gamma 90.00 _cell_volume 5161.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 0.815 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.709492 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12559 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.1063 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9356 _reflns_number_gt 5844 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1157P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(5) _refine_ls_number_reflns 9356 _refine_ls_number_parameters 597 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.2047 _refine_ls_wR_factor_gt 0.1781 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.179 _refine_ls_shift/su_mean 0.013 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 Ag1 Ag 0.55844(4) 0.43333(9) -0.01520(3) 0.0493(2) Uani 1 1 d . . . Ag2 Ag 0.5000 0.56695(12) 0.5000 0.0546(4) Uani 1 2 d S . . P1 P 0.61925(12) 0.3349(3) 0.06841(10) 0.0416(6) Uani 1 1 d . . . P2 P 0.39064(12) 0.6001(3) 0.43736(10) 0.0445(7) Uani 1 1 d . . . N1 N 0.4848(4) 0.5104(10) 0.0992(4) 0.050(2) Uani 1 1 d . . . N2 N 0.5081(4) 0.2811(9) 0.0965(3) 0.0407(19) Uani 1 1 d . . . C1 C 0.6631(5) 0.4585(13) 0.1207(4) 0.051(3) Uani 1 1 d . . . C2 C 0.7038(5) 0.4177(18) 0.1691(4) 0.066(3) Uani 1 1 d . . . H2A H 0.7104 0.3219 0.1754 0.079 Uiso 1 1 calc R . . C3 C 0.7348(7) 0.5049(18) 0.2081(6) 0.078(4) Uani 1 1 d . . . H3A H 0.7624 0.4716 0.2408 0.094 Uiso 1 1 calc R . . C4 C 0.7247(7) 0.647(2) 0.1986(8) 0.090(5) Uani 1 1 d . . . H4A H 0.7462 0.7111 0.2251 0.108 Uiso 1 1 calc R . . C5 C 0.6839(8) 0.6950(16) 0.1512(7) 0.088(5) Uani 1 1 d . . . H5A H 0.6774 0.7910 0.1454 0.105 Uiso 1 1 calc R . . C6 C 0.6517(6) 0.6015(12) 0.1114(5) 0.056(3) Uani 1 1 d . . . H6A H 0.6229 0.6336 0.0789 0.067 Uiso 1 1 calc R . . C7 C 0.6847(5) 0.2231(11) 0.0625(4) 0.043(2) Uani 1 1 d . . . C8 C 0.6845(6) 0.0836(13) 0.0648(5) 0.062(3) Uani 1 1 d . . . H8A H 0.6500 0.0385 0.0719 0.074 Uiso 1 1 calc R . . C9 C 0.7370(7) -0.0008(16) 0.0564(6) 0.079(4) Uani 1 1 d . . . H9A H 0.7360 -0.0983 0.0567 0.095 Uiso 1 1 calc R . . C10 C 0.7877(7) 0.0716(18) 0.0483(5) 0.075(4) Uani 1 1 d . . . H10A H 0.8226 0.0217 0.0436 0.090 Uiso 1 1 calc R . . C11 C 0.7887(6) 0.2112(19) 0.0467(5) 0.077(4) Uani 1 1 d . . . H11A H 0.8235 0.2563 0.0401 0.092 Uiso 1 1 calc R . . C12 C 0.7390(6) 0.2902(15) 0.0546(5) 0.064(3) Uani 1 1 d . . . H12A H 0.7414 0.3876 0.0547 0.077 Uiso 1 1 calc R . . C13 C 0.5728(5) 0.2146(10) 0.0969(4) 0.040(2) Uani 1 1 d . . . H13A H 0.5632 0.1282 0.0767 0.048 Uiso 1 1 calc R . . H13B H 0.6000 0.1917 0.1330 0.048 Uiso 1 1 calc R . . C14 C 0.5172(5) 0.4010(11) 0.1285(4) 0.043(3) Uani 1 1 d . . . C15 C 0.5527(5) 0.4113(13) 0.1799(4) 0.053(3) Uani 1 1 d . . . H15A H 0.5721 0.3321 0.1993 0.064 Uiso 1 1 calc R . . C16 C 0.5603(6) 0.5421(16) 0.2040(5) 0.067(4) Uani 1 1 d . . . H16A H 0.5866 0.5516 0.2394 0.081 Uiso 1 1 calc R . . C17 C 0.5300(7) 0.6540(14) 0.1766(5) 0.068(4) Uani 1 1 d . . . H17A H 0.5341 0.7425 0.1920 0.081 Uiso 1 1 calc R . . C18 C 0.4911(6) 0.6314(14) 0.1227(6) 0.064(3) Uani 1 1 d . . . H18A H 0.4687 0.7077 0.1030 0.077 Uiso 1 1 calc R . . C19 C 0.4611(5) 0.1689(12) 0.1044(6) 0.059(3) Uani 1 1 d . . . H19A H 0.4557 0.0990 0.0766 0.071 Uiso 1 1 calc R . . C20 C 0.4826(6) 0.0919(15) 0.1539(6) 0.073(4) Uani 1 1 d . . . H20A H 0.4899 0.1574 0.1829 0.087 Uiso 1 1 calc R . . H20B H 0.5247 0.0463 0.1583 0.087 Uiso 1 1 calc R . . C21 C 0.4338(7) -0.0154(14) 0.1565(7) 0.081(4) Uani 1 1 d . . . H21A H 0.4497 -0.0596 0.1911 0.097 Uiso 1 1 calc R . . H21B H 0.4306 -0.0873 0.1303 0.097 Uiso 1 1 calc R . . C22 C 0.3660(6) 0.0439(15) 0.1471(5) 0.068(4) Uani 1 1 d . . . H22A H 0.3351 -0.0315 0.1460 0.081 Uiso 1 1 calc R . . H22B H 0.3674 0.1063 0.1759 0.081 Uiso 1 1 calc R . . C23 C 0.3430(6) 0.1216(14) 0.0969(7) 0.077(4) Uani 1 1 d . . . H23A H 0.3007 0.1658 0.0928 0.093 Uiso 1 1 calc R . . H23B H 0.3356 0.0558 0.0679 0.093 Uiso 1 1 calc R . . C24 C 0.3925(5) 0.2348(13) 0.0932(5) 0.058(3) Uani 1 1 d . . . H24A H 0.3771 0.2760 0.0581 0.070 Uiso 1 1 calc R . . H24B H 0.3952 0.3086 0.1186 0.070 Uiso 1 1 calc R . . N3 N 0.5015(5) 0.3622(10) 0.4340(4) 0.063(3) Uani 1 1 d . . . N4 N 0.4363(4) 0.4852(9) 0.3608(3) 0.045(2) Uani 1 1 d . . . C25 C 0.3630(6) 0.7715(15) 0.4090(4) 0.056(3) Uani 1 1 d . . . C26 C 0.4066(7) 0.8828(13) 0.4222(5) 0.065(3) Uani 1 1 d . . . H26A H 0.4503 0.8690 0.4445 0.078 Uiso 1 1 calc R . . C27 C 0.3856(10) 1.0150(17) 0.4023(6) 0.093(5) Uani 1 1 d . . . H27A H 0.4150 1.0899 0.4131 0.111 Uiso 1 1 calc R . . C28 C 0.3235(12) 1.0386(18) 0.3677(7) 0.104(6) Uani 1 1 d . . . H28A H 0.3113 1.1262 0.3522 0.124 Uiso 1 1 calc R . . C29 C 0.2785(8) 0.927(2) 0.3560(5) 0.088(5) Uani 1 1 d . . . H29A H 0.2346 0.9426 0.3345 0.105 Uiso 1 1 calc R . . C30 C 0.2981(6) 0.7947(13) 0.3761(4) 0.052(3) Uani 1 1 d . . . H30A H 0.2678 0.7210 0.3674 0.062 Uiso 1 1 calc R . . C31 C 0.3256(5) 0.5442(11) 0.4618(4) 0.044(2) Uani 1 1 d . . . C32 C 0.3310(6) 0.5764(15) 0.5127(4) 0.062(3) Uani 1 1 d . . . H32A H 0.3677 0.6264 0.5340 0.075 Uiso 1 1 calc R . . C33 C 0.2814(10) 0.5344(19) 0.5328(7) 0.100(6) Uani 1 1 d . . . H33A H 0.2854 0.5580 0.5673 0.120 Uiso 1 1 calc R . . C34 C 0.2295(8) 0.4621(18) 0.5033(7) 0.088(5) Uani 1 1 d . . . H34A H 0.1975 0.4333 0.5173 0.105 Uiso 1 1 calc R . . C35 C 0.2227(6) 0.431(2) 0.4547(6) 0.087(4) Uani 1 1 d . . . H35A H 0.1854 0.3811 0.4339 0.104 Uiso 1 1 calc R . . C36 C 0.2710(6) 0.4708(14) 0.4338(5) 0.070(4) Uani 1 1 d . . . H36A H 0.2653 0.4461 0.3991 0.083 Uiso 1 1 calc R . . C37 C 0.3823(5) 0.4808(12) 0.3823(4) 0.049(3) Uani 1 1 d . . . H37A H 0.3788 0.3857 0.3939 0.059 Uiso 1 1 calc R . . H37B H 0.3409 0.5022 0.3540 0.059 Uiso 1 1 calc R . . C38 C 0.4927(6) 0.4025(11) 0.3857(4) 0.054(3) Uani 1 1 d . . . C39 C 0.5375(7) 0.3661(17) 0.3616(7) 0.089(5) Uani 1 1 d . . . H39A H 0.5311 0.3974 0.3275 0.107 Uiso 1 1 calc R . . C40 C 0.5901(9) 0.2861(19) 0.3867(7) 0.102(6) Uani 1 1 d . . . H40A H 0.6182 0.2555 0.3692 0.122 Uiso 1 1 calc R . . C41 C 0.6025(8) 0.249(2) 0.4393(9) 0.108(6) Uani 1 1 d . . . H41A H 0.6407 0.2008 0.4594 0.130 Uiso 1 1 calc R . . C42 C 0.5561(7) 0.2861(15) 0.4584(6) 0.087(5) Uani 1 1 d . . . H42A H 0.5620 0.2565 0.4926 0.104 Uiso 1 1 calc R . . C43 C 0.4198(5) 0.5288(12) 0.3056(4) 0.051(3) Uani 1 1 d . . . H43A H 0.4622 0.5411 0.2999 0.061 Uiso 1 1 calc R . . C44 C 0.3817(6) 0.4198(16) 0.2666(4) 0.072(4) Uani 1 1 d . . . H44A H 0.3391 0.4041 0.2708 0.087 Uiso 1 1 calc R . . H44B H 0.4062 0.3321 0.2739 0.087 Uiso 1 1 calc R . . C45 C 0.3703(7) 0.4645(17) 0.2093(5) 0.078(4) Uani 1 1 d . . . H45A H 0.4126 0.4682 0.2037 0.094 Uiso 1 1 calc R . . H45B H 0.3426 0.3954 0.1852 0.094 Uiso 1 1 calc R . . C46 C 0.3384(9) 0.601(2) 0.1981(5) 0.108(6) Uani 1 1 d . . . H46A H 0.2938 0.5934 0.1994 0.129 Uiso 1 1 calc R . . H46B H 0.3345 0.6289 0.1626 0.129 Uiso 1 1 calc R . . C47 C 0.3753(8) 0.7089(17) 0.2357(5) 0.082(4) Uani 1 1 d . . . H47A H 0.3512 0.7970 0.2274 0.098 Uiso 1 1 calc R . . H47B H 0.4185 0.7227 0.2322 0.098 Uiso 1 1 calc R . . C48 C 0.3848(7) 0.6665(13) 0.2933(4) 0.061(3) Uani 1 1 d . . . H48A H 0.4107 0.7375 0.3175 0.074 Uiso 1 1 calc R . . H48B H 0.3418 0.6596 0.2977 0.074 Uiso 1 1 calc R . . Cl1 Cl 0.3320(2) 0.0291(5) 0.74022(15) 0.0891(12) Uani 1 1 d . . . O1 O 0.2765(6) -0.0327(17) 0.7070(5) 0.137(5) Uani 1 1 d . . . O2 O 0.3833(7) -0.060(2) 0.7534(8) 0.205(8) Uani 1 1 d . . . O3 O 0.3480(11) 0.142(2) 0.7178(10) 0.241(12) Uani 1 1 d . . . O4 O 0.3275(11) 0.055(3) 0.7871(7) 0.263(15) Uani 1 1 d . . . Cl2 Cl 0.0000 0.3313(6) 0.0000 0.118(2) Uani 1 2 d S . . O5 O -0.0490(9) 0.2417(14) 0.0109(5) 0.188(9) Uani 1 1 d . . . O6 O 0.0306(10) 0.3914(18) 0.0475(9) 0.244(11) Uani 1 1 d . . . C49 C 0.5581(14) 0.962(2) 0.3381(15) 0.20(3) Uani 0.50 1 d PD . . H49A H 0.5818 0.9642 0.3132 0.245 Uiso 0.50 1 calc PR . . H49B H 0.5808 1.0233 0.3676 0.245 Uiso 0.50 1 calc PR . . Cl3 Cl 0.4757(12) 1.0154(17) 0.3075(7) 0.228(9) Uani 0.50 1 d PD . . Cl4 Cl 0.5534(8) 0.792(2) 0.3598(9) 0.296(15) Uani 0.50 1 d PD . . 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 Ag1 0.0322(4) 0.0699(5) 0.0461(4) 0.0050(5) 0.0141(3) 0.0023(4) Ag2 0.0391(7) 0.0703(9) 0.0419(6) 0.000 -0.0020(5) 0.000 P1 0.0296(13) 0.0501(16) 0.0444(14) -0.0006(13) 0.0118(11) 0.0013(12) P2 0.0333(14) 0.0591(18) 0.0363(13) 0.0003(12) 0.0061(11) -0.0007(12) N1 0.035(5) 0.053(6) 0.060(6) -0.007(5) 0.016(4) 0.006(4) N2 0.032(4) 0.053(5) 0.039(4) -0.007(4) 0.015(4) -0.011(4) C1 0.028(5) 0.070(8) 0.062(7) 0.013(6) 0.025(5) 0.015(5) C2 0.043(6) 0.104(10) 0.052(6) -0.021(8) 0.019(5) -0.018(8) C3 0.056(8) 0.105(12) 0.068(8) -0.035(8) 0.016(7) -0.014(8) C4 0.047(8) 0.109(14) 0.110(13) -0.043(11) 0.022(9) -0.020(8) C5 0.077(10) 0.068(9) 0.126(14) -0.036(10) 0.046(11) -0.020(8) C6 0.047(6) 0.054(7) 0.072(8) -0.008(6) 0.027(6) -0.008(6) C7 0.044(6) 0.039(6) 0.045(6) -0.008(5) 0.014(5) 0.002(5) C8 0.063(8) 0.050(7) 0.087(9) -0.007(7) 0.044(7) -0.007(6) C9 0.053(8) 0.079(9) 0.102(11) -0.008(8) 0.023(8) 0.024(7) C10 0.062(9) 0.095(11) 0.080(9) -0.001(9) 0.039(7) 0.033(9) C11 0.031(6) 0.123(14) 0.077(9) -0.009(9) 0.019(6) 0.014(7) C12 0.060(8) 0.073(8) 0.069(8) 0.000(7) 0.035(7) 0.013(7) C13 0.038(6) 0.036(5) 0.052(6) 0.000(5) 0.022(5) 0.011(5) C14 0.028(5) 0.056(7) 0.051(6) -0.001(5) 0.022(4) -0.006(5) C15 0.046(6) 0.059(8) 0.053(6) -0.008(6) 0.014(5) 0.010(6) C16 0.043(7) 0.094(10) 0.059(7) -0.020(8) 0.008(6) 0.000(7) C17 0.064(8) 0.058(8) 0.084(10) -0.031(7) 0.029(8) -0.010(7) C18 0.051(8) 0.059(8) 0.090(10) -0.020(7) 0.033(7) -0.011(6) C19 0.039(6) 0.050(7) 0.095(9) -0.005(7) 0.033(6) 0.002(5) C20 0.050(7) 0.079(9) 0.095(10) 0.036(8) 0.032(7) 0.004(7) C21 0.061(8) 0.078(9) 0.113(11) 0.034(8) 0.042(8) 0.000(7) C22 0.050(7) 0.084(9) 0.084(9) 0.029(8) 0.042(7) 0.009(7) C23 0.048(7) 0.070(8) 0.123(12) 0.011(8) 0.041(8) 0.005(6) C24 0.031(6) 0.065(7) 0.079(8) 0.004(6) 0.019(6) 0.006(5) N3 0.063(6) 0.059(6) 0.056(6) -0.004(5) 0.004(5) 0.014(5) N4 0.037(5) 0.054(5) 0.044(5) -0.006(4) 0.013(4) 0.005(4) C25 0.058(8) 0.077(9) 0.036(6) -0.002(6) 0.019(6) 0.000(7) C26 0.077(9) 0.064(8) 0.052(7) -0.003(6) 0.019(7) -0.002(7) C27 0.111(14) 0.068(10) 0.075(10) -0.001(8) 0.003(10) -0.018(9) C28 0.18(2) 0.061(10) 0.085(12) 0.010(9) 0.060(14) 0.021(12) C29 0.092(10) 0.109(12) 0.062(8) 0.016(10) 0.027(7) 0.056(12) C30 0.046(6) 0.062(7) 0.044(6) 0.010(6) 0.012(5) 0.008(5) C31 0.038(5) 0.047(6) 0.045(5) 0.010(5) 0.012(4) 0.012(5) C32 0.049(7) 0.090(9) 0.050(6) -0.004(7) 0.021(5) -0.006(7) C33 0.126(15) 0.118(14) 0.074(10) 0.030(10) 0.058(11) 0.007(12) C34 0.076(10) 0.107(13) 0.094(11) 0.027(10) 0.047(9) -0.016(9) C35 0.049(7) 0.119(12) 0.091(10) 0.029(12) 0.025(7) -0.022(9) C36 0.055(7) 0.089(11) 0.060(7) 0.005(7) 0.014(6) -0.001(7) C37 0.039(6) 0.058(7) 0.043(5) 0.001(5) 0.005(5) -0.007(5) C38 0.049(6) 0.050(7) 0.054(6) -0.012(5) 0.008(5) -0.003(5) C39 0.049(8) 0.120(13) 0.099(11) -0.022(9) 0.026(8) 0.027(8) C40 0.085(12) 0.110(13) 0.096(12) -0.038(11) 0.014(10) 0.023(10) C41 0.056(9) 0.120(14) 0.139(17) -0.001(13) 0.021(11) 0.041(10) C42 0.071(10) 0.070(9) 0.085(10) -0.010(8) -0.016(8) 0.025(8) C43 0.040(6) 0.068(8) 0.046(6) -0.003(5) 0.017(5) 0.005(5) C44 0.060(7) 0.090(9) 0.060(7) -0.025(8) 0.011(6) 0.013(8) C45 0.072(9) 0.103(12) 0.060(7) -0.017(8) 0.023(7) 0.006(8) C46 0.097(12) 0.184(19) 0.032(6) -0.006(10) 0.008(7) 0.022(13) C47 0.088(10) 0.103(11) 0.064(8) 0.023(8) 0.038(8) 0.016(9) C48 0.068(8) 0.072(8) 0.048(6) 0.000(6) 0.024(6) 0.005(7) Cl1 0.067(2) 0.117(3) 0.065(2) -0.003(2) -0.0009(18) 0.008(2) O1 0.092(8) 0.185(14) 0.094(8) -0.028(9) -0.019(7) -0.011(9) O2 0.099(10) 0.215(16) 0.240(19) -0.051(18) -0.019(11) 0.025(14) O3 0.198(19) 0.148(14) 0.29(3) 0.083(16) -0.025(18) -0.078(14) O4 0.191(19) 0.47(4) 0.132(14) -0.12(2) 0.059(13) -0.08(2) Cl2 0.144(6) 0.046(3) 0.152(6) 0.000 0.037(5) 0.000 O5 0.262(18) 0.144(11) 0.070(7) 0.049(8) -0.057(10) -0.131(12) O6 0.26(2) 0.163(15) 0.37(3) -0.190(17) 0.19(2) -0.148(16) C49 0.28(7) 0.16(5) 0.08(2) -0.04(3) -0.05(3) 0.10(5) Cl3 0.35(3) 0.146(11) 0.187(15) -0.026(11) 0.096(18) -0.081(15) Cl4 0.142(12) 0.30(2) 0.32(3) 0.13(2) -0.082(14) -0.121(15) _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 Ag1 N1 2.252(9) 2_655 ? Ag1 P1 2.372(3) . ? Ag1 N2 2.603(8) 2_655 ? Ag1 Ag1 2.8898(15) 2_655 ? Ag2 P2 2.388(2) . ? Ag2 P2 2.388(2) 2_656 ? P1 C7 1.810(10) . ? P1 C1 1.828(12) . ? P1 C13 1.850(10) . ? P2 C31 1.814(11) . ? P2 C25 1.814(14) . ? P2 C37 1.829(11) . ? N1 C18 1.300(14) . ? N1 C14 1.347(13) . ? N1 Ag1 2.252(9) 2_655 ? N2 C14 1.405(13) . ? N2 C13 1.520(12) . ? N2 C19 1.533(14) . ? N2 Ag1 2.603(8) 2_655 ? C1 C2 1.351(15) . ? C1 C6 1.393(16) . ? C2 C3 1.325(17) . ? C3 C4 1.39(2) . ? C4 C5 1.35(2) . ? C5 C6 1.382(18) . ? C7 C8 1.331(16) . ? C7 C12 1.407(16) . ? C8 C9 1.462(17) . ? C9 C10 1.37(2) . ? C10 C11 1.33(2) . ? C11 C12 1.378(17) . ? C14 C15 1.332(14) . ? C15 C16 1.389(17) . ? C16 C17 1.331(18) . ? C17 C18 1.419(18) . ? C19 C20 1.451(17) . ? C19 C24 1.529(14) . ? C20 C21 1.482(17) . ? C21 C22 1.496(17) . ? C22 C23 1.471(18) . ? C23 C24 1.540(16) . ? N3 C38 1.308(14) . ? N3 C42 1.340(16) . ? N4 C38 1.404(13) . ? N4 C37 1.461(13) . ? N4 C43 1.467(13) . ? C25 C26 1.375(18) . ? C25 C30 1.384(16) . ? C26 C27 1.382(19) . ? C27 C28 1.35(2) . ? C28 C29 1.39(2) . ? C29 C30 1.38(2) . ? C31 C36 1.349(16) . ? C31 C32 1.370(14) . ? C32 C33 1.408(19) . ? C33 C34 1.32(2) . ? C34 C35 1.30(2) . ? C35 C36 1.392(17) . ? C38 C39 1.377(17) . ? C39 C40 1.33(2) . ? C40 C41 1.40(2) . ? C41 C42 1.31(2) . ? C43 C48 1.491(16) . ? C43 C44 1.502(17) . ? C44 C45 1.537(17) . ? C45 C46 1.45(2) . ? C46 C47 1.47(2) . ? C47 C48 1.549(17) . ? Cl1 O3 1.336(18) . ? Cl1 O4 1.324(16) . ? Cl1 O2 1.338(18) . ? Cl1 O1 1.351(12) . ? Cl2 O6 1.347(18) 2 ? Cl2 O6 1.347(18) . ? Cl2 O5 1.459(14) 2 ? Cl2 O5 1.459(14) . ? C49 Cl4 1.738(10) . ? C49 Cl3 1.745(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 N1 Ag1 P1 169.7(2) 2_655 . ? N1 Ag1 N2 54.6(3) 2_655 2_655 ? P1 Ag1 N2 122.68(19) . 2_655 ? N1 Ag1 Ag1 100.9(2) 2_655 2_655 ? P1 Ag1 Ag1 88.60(7) . 2_655 ? N2 Ag1 Ag1 87.87(17) 2_655 2_655 ? P2 Ag2 P2 164.81(15) . 2_656 ? C7 P1 C1 103.9(5) . . ? C7 P1 C13 102.4(5) . . ? C1 P1 C13 106.6(5) . . ? C7 P1 Ag1 109.7(4) . . ? C1 P1 Ag1 116.4(4) . . ? C13 P1 Ag1 116.3(3) . . ? C31 P2 C25 103.8(5) . . ? C31 P2 C37 103.9(5) . . ? C25 P2 C37 107.0(5) . . ? C31 P2 Ag2 113.1(3) . . ? C25 P2 Ag2 120.9(4) . . ? C37 P2 Ag2 106.8(4) . . ? C18 N1 C14 117.1(10) . . ? C18 N1 Ag1 135.8(9) . 2_655 ? C14 N1 Ag1 106.7(7) . 2_655 ? C14 N2 C13 113.6(7) . . ? C14 N2 C19 116.1(8) . . ? C13 N2 C19 110.4(8) . . ? C14 N2 Ag1 89.1(6) . 2_655 ? C13 N2 Ag1 118.2(6) . 2_655 ? C19 N2 Ag1 108.2(6) . 2_655 ? C2 C1 C6 118.0(12) . . ? C2 C1 P1 123.1(11) . . ? C6 C1 P1 118.7(8) . . ? C3 C2 C1 124.4(16) . . ? C2 C3 C4 117.7(16) . . ? C5 C4 C3 120.8(15) . . ? C4 C5 C6 120.2(15) . . ? C5 C6 C1 118.8(13) . . ? C8 C7 C12 118.5(10) . . ? C8 C7 P1 124.7(9) . . ? C12 C7 P1 116.8(8) . . ? C7 C8 C9 121.8(12) . . ? C10 C9 C8 116.3(13) . . ? C11 C10 C9 122.1(12) . . ? C10 C11 C12 121.3(14) . . ? C11 C12 C7 119.9(13) . . ? N2 C13 P1 111.0(6) . . ? C15 C14 N1 123.1(10) . . ? C15 C14 N2 127.4(10) . . ? N1 C14 N2 109.5(8) . . ? C14 C15 C16 118.9(11) . . ? C17 C16 C15 120.3(11) . . ? C16 C17 C18 116.5(12) . . ? N1 C18 C17 124.0(13) . . ? C20 C19 C24 111.6(10) . . ? C20 C19 N2 117.8(10) . . ? C24 C19 N2 108.6(9) . . ? C19 C20 C21 112.8(12) . . ? C20 C21 C22 113.0(11) . . ? C23 C22 C21 110.1(10) . . ? C22 C23 C24 113.1(12) . . ? C19 C24 C23 109.6(10) . . ? C38 N3 C42 116.6(13) . . ? C38 N4 C37 117.6(9) . . ? C38 N4 C43 120.6(9) . . ? C37 N4 C43 117.6(8) . . ? C26 C25 C30 118.9(13) . . ? C26 C25 P2 119.5(10) . . ? C30 C25 P2 121.5(10) . . ? C25 C26 C27 120.1(14) . . ? C28 C27 C26 122.0(15) . . ? C27 C28 C29 117.8(14) . . ? C30 C29 C28 120.9(14) . . ? C29 C30 C25 120.0(13) . . ? C36 C31 C32 115.7(11) . . ? C36 C31 P2 125.1(9) . . ? C32 C31 P2 119.2(9) . . ? C31 C32 C33 120.6(13) . . ? C34 C33 C32 120.5(14) . . ? C35 C34 C33 120.4(14) . . ? C34 C35 C36 120.3(14) . . ? C31 C36 C35 122.5(13) . . ? N4 C37 P2 115.7(7) . . ? N3 C38 C39 120.9(12) . . ? N3 C38 N4 116.4(10) . . ? C39 C38 N4 122.7(11) . . ? C40 C39 C38 120.5(17) . . ? C39 C40 C41 119.5(17) . . ? C42 C41 C40 115.1(16) . . ? C41 C42 N3 127.2(17) . . ? N4 C43 C48 113.6(9) . . ? N4 C43 C44 113.4(10) . . ? C48 C43 C44 110.2(10) . . ? C43 C44 C45 111.8(12) . . ? C46 C45 C44 110.9(12) . . ? C45 C46 C47 112.5(12) . . ? C46 C47 C48 111.1(13) . . ? C43 C48 C47 109.5(10) . . ? O3 Cl1 O4 113.1(18) . . ? O3 Cl1 O2 108.6(16) . . ? O4 Cl1 O2 101.0(15) . . ? O3 Cl1 O1 110.8(11) . . ? O4 Cl1 O1 112.3(12) . . ? O2 Cl1 O1 110.6(11) . . ? O6 Cl2 O6 130(2) 2 . ? O6 Cl2 O5 101.9(9) 2 2 ? O6 Cl2 O5 107.0(10) . 2 ? O6 Cl2 O5 107.0(10) 2 . ? O6 Cl2 O5 101.9(9) . . ? O5 Cl2 O5 108.4(16) 2 . ? Cl4 C49 Cl3 105.2(17) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.188 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.122 #===============================================END