Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Yong-Joo Kim' 'Jin-Taek Han' 'Won Seok Han' 'Seok Kang' 'Soon Lee' _publ_contact_author_name 'Prof Yong-Joo Kim' _publ_contact_author_address ; Department of Chemistry Kangnung National University Kangnung 210-702 KOREA ; _publ_contact_author_email YJKIM@KNUSUN.KANGNUNG.AC.KR _publ_section_title ; Reactivity of bis(azido)bis(phosphine) complexes of Ni(II), Pd(II), and Pt(II) toward organic isothiocyanates: synthesis, structures, and properties of M{S[CN4(R)]}2L2 and M(NCS)2L2 (M = Ni, Pd, Pt; R= allyl, benzyl, ethyl, phenyl, 2,6-dimethylphenyl; L = PMe3, PEt3, PMe2Ph, L-L = depe ; data_ni(ncs)2 _database_code_CSD 210413 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H18 N2 Ni P2 S2' _chemical_formula_weight 327.01 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 6.1832(13) _cell_length_b 7.2920(11) _cell_length_c 16.744(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.906(16) _cell_angle_gamma 90.00 _cell_volume 754.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.03 _cell_measurement_theta_max 14.08 _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2464 _exptl_absorpt_correction_T_max 0.2892 _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 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1458 _diffrn_reflns_av_R_equivalents 0.0122 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1329 _reflns_number_gt 1235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0268P)^2^+0.1848P] 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 0.0105(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1329 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Ni1 Ni 0.0000 0.0000 0.0000 0.04015(15) Uani 1 2 d S . . P1 P 0.01851(8) 0.15189(7) -0.11508(3) 0.03942(16) Uani 1 1 d . . . S1 S -0.61936(9) -0.29363(9) -0.09221(4) 0.0604(2) Uani 1 1 d . . . N1 N -0.2394(3) -0.1257(2) -0.03743(10) 0.0485(4) Uani 1 1 d . . . C1 C -0.3975(3) -0.1963(3) -0.05999(11) 0.0418(4) Uani 1 1 d . . . C2 C -0.1174(4) 0.0439(4) -0.19997(13) 0.0652(7) Uani 1 1 d . . . H2A H -0.0622 -0.0780 -0.2064 0.078 Uiso 1 1 calc R . . H2B H -0.0923 0.1140 -0.2473 0.078 Uiso 1 1 calc R . . H2C H -0.2700 0.0384 -0.1913 0.078 Uiso 1 1 calc R . . C3 C -0.0979(4) 0.3786(3) -0.10927(14) 0.0614(6) Uani 1 1 d . . . H3A H -0.0324 0.4434 -0.0648 0.074 Uiso 1 1 calc R . . H3B H -0.2509 0.3686 -0.1022 0.074 Uiso 1 1 calc R . . H3C H -0.0724 0.4442 -0.1578 0.074 Uiso 1 1 calc R . . C4 C 0.2874(4) 0.1959(4) -0.14960(16) 0.0634(6) Uani 1 1 d . . . H4A H 0.3727 0.2536 -0.1077 0.076 Uiso 1 1 calc R . . H4B H 0.2785 0.2753 -0.1953 0.076 Uiso 1 1 calc R . . H4C H 0.3539 0.0822 -0.1641 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0354(2) 0.0430(2) 0.0416(2) 0.00446(14) -0.00603(15) -0.01248(14) P1 0.0329(3) 0.0461(3) 0.0392(3) 0.0028(2) 0.0001(2) -0.0054(2) S1 0.0459(3) 0.0595(4) 0.0750(4) -0.0113(3) -0.0090(3) -0.0182(3) N1 0.0432(10) 0.0517(10) 0.0500(10) 0.0047(8) -0.0067(8) -0.0141(8) C1 0.0420(11) 0.0406(10) 0.0427(10) -0.0002(8) 0.0015(8) -0.0053(9) C2 0.0643(15) 0.0921(18) 0.0395(11) -0.0101(12) 0.0045(11) -0.0226(14) C3 0.0633(15) 0.0585(14) 0.0622(14) 0.0068(11) -0.0005(12) 0.0099(12) C4 0.0405(12) 0.0720(16) 0.0782(16) 0.0181(13) 0.0113(11) -0.0047(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.8340(17) 3 ? Ni1 N1 1.8340(17) . ? Ni1 P1 2.2287(6) 3 ? Ni1 P1 2.2287(6) . ? P1 C4 1.807(2) . ? P1 C3 1.807(2) . ? P1 C2 1.808(2) . ? S1 C1 1.621(2) . ? N1 C1 1.157(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 Ni1 N1 180.00(15) 3 . ? N1 Ni1 P1 90.98(6) 3 3 ? N1 Ni1 P1 89.02(6) . 3 ? N1 Ni1 P1 89.02(6) 3 . ? N1 Ni1 P1 90.98(6) . . ? P1 Ni1 P1 180.00(3) 3 . ? C4 P1 C3 103.13(12) . . ? C4 P1 C2 103.57(13) . . ? C3 P1 C2 105.37(13) . . ? C4 P1 Ni1 116.04(9) . . ? C3 P1 Ni1 112.09(8) . . ? C2 P1 Ni1 115.31(9) . . ? C1 N1 Ni1 176.07(19) . . ? N1 C1 S1 179.4(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.220 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.043 #=====================================================END data_abspt _database_code_CSD 210414 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H32 N2 O P2 Pt S2' _chemical_formula_weight 565.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/nmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y, z' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 12.207(2) _cell_length_b 12.207(2) _cell_length_c 16.112(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2401.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 5.37 _cell_measurement_theta_max 12.44 _exptl_crystal_description 'CUBE ' _exptl_crystal_colour 'COLORLESS ' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 6.154 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2659 _exptl_absorpt_correction_T_max 0.2832 _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 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1156 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1155 _reflns_number_gt 708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0377P)^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 0.00044(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1155 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.214 _refine_ls_shift/su_mean 0.012 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.2500 0.2500 0.22703(3) 0.0430(2) Uani 1 4 d S . . S1 S -0.0271(3) 0.2500 0.4386(2) 0.0631(9) Uani 1 2 d S . . P1 P 0.3965(3) 0.2500 0.14089(19) 0.0417(7) Uani 1 2 d S . . N1 N 0.1338(9) 0.2500 0.3197(6) 0.064(3) Uani 1 2 d S . . C1 C 0.3837(10) 0.2500 0.0279(6) 0.049(3) Uani 1 2 d S . . H1A H 0.3420 0.1859 0.0115 0.059 Uiso 0.50 1 calc PR . . H1B H 0.3420 0.3141 0.0115 0.059 Uiso 0.50 1 calc PR . . C2 C 0.4915(12) 0.2500 -0.0196(7) 0.077(4) Uani 1 2 d S . . H2A H 0.4769 0.2500 -0.0781 0.092 Uiso 1 2 calc SR . . H2B H 0.5328 0.1858 -0.0052 0.092 Uiso 0.50 1 calc PR . . H2C H 0.5328 0.3142 -0.0052 0.092 Uiso 0.50 1 calc PR . . C3 C 0.4825(7) 0.3686(7) 0.1631(5) 0.056(2) Uani 1 1 d . . . H3A H 0.5035 0.3663 0.2212 0.067 Uiso 1 1 calc R . . H3B H 0.5489 0.3630 0.1304 0.067 Uiso 1 1 calc R . . C4 C 0.4301(9) 0.4764(8) 0.1458(6) 0.086(4) Uani 1 1 d . . . H4A H 0.4803 0.5343 0.1593 0.104 Uiso 1 1 calc R . . H4B H 0.3651 0.4838 0.1789 0.104 Uiso 1 1 calc R . . H4C H 0.4110 0.4807 0.0881 0.104 Uiso 1 1 calc R . . C5 C 0.0657(10) 0.2500 0.3679(7) 0.044(3) Uani 1 2 d S . . O1 O 0.2500 0.7500 0.1559(14) 0.147(8) Uani 1 4 d S . . HO1 H 0.311(11) 0.7500 0.210(6) 0.080 Uiso 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0437(5) 0.0495(6) 0.0358(3) 0.000 0.000 0.000 S1 0.060(2) 0.071(2) 0.0574(18) 0.000 0.014(2) 0.000 P1 0.0361(16) 0.0468(18) 0.0421(15) 0.000 0.0001(14) 0.000 N1 0.057(7) 0.096(9) 0.040(5) 0.000 0.008(6) 0.000 C1 0.047(7) 0.057(7) 0.043(6) 0.000 0.002(6) 0.000 C2 0.070(10) 0.108(12) 0.053(8) 0.000 0.013(8) 0.000 C3 0.045(5) 0.064(6) 0.059(5) -0.004(5) -0.002(4) -0.013(5) C4 0.097(9) 0.068(6) 0.094(7) 0.011(6) -0.032(6) -0.014(7) C5 0.045(7) 0.050(7) 0.036(6) 0.000 -0.011(6) 0.000 O1 0.18(2) 0.073(12) 0.19(2) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.059(10) 2 ? Pt1 N1 2.059(10) . ? Pt1 P1 2.263(3) . ? Pt1 P1 2.263(3) 2 ? S1 C5 1.607(12) . ? P1 C3 1.824(8) . ? P1 C3 1.824(8) 13_565 ? P1 C1 1.827(10) . ? N1 C5 1.138(13) . ? C1 C2 1.522(17) . ? C3 C4 1.490(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N1 87.1(6) 2 . ? N1 Pt1 P1 84.3(3) 2 . ? N1 Pt1 P1 171.4(3) . . ? N1 Pt1 P1 171.4(3) 2 2 ? N1 Pt1 P1 84.3(3) . 2 ? P1 Pt1 P1 104.36(16) . 2 ? C3 P1 C3 105.1(6) . 13_565 ? C3 P1 C1 104.2(4) . . ? C3 P1 C1 104.2(4) 13_565 . ? C3 P1 Pt1 109.5(3) . . ? C3 P1 Pt1 109.5(3) 13_565 . ? C1 P1 Pt1 122.9(4) . . ? C5 N1 Pt1 176.6(10) . . ? C2 C1 P1 115.2(8) . . ? C4 C3 P1 114.6(6) . . ? N1 C5 S1 177.9(10) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.862 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.119 #==============================================================END data_2sallyl _database_code_CSD 210415 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H28 N8 P2 Pd S2' _chemical_formula_weight 540.90 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' S S 0.1246 0.1234 '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 'P2(1)/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 12.015(2) _cell_length_b 8.3887(4) _cell_length_c 11.8788(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.749(10) _cell_angle_gamma 90.00 _cell_volume 1188.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 7.05 _cell_measurement_theta_max 12.52 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0319 _exptl_absorpt_correction_T_max 0.0536 _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 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2186 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2075 _reflns_number_gt 1997 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0409P)^2^+0.5467P] 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 0.0021(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2075 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.004 _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 0.0000 0.0000 0.0000 0.04504(13) Uani 1 2 d S . . P1 P -0.10050(6) 0.14991(8) 0.11794(6) 0.05423(18) Uani 1 1 d . . . S1 S 0.13684(6) 0.19991(8) 0.02192(6) 0.05873(19) Uani 1 1 d . . . N1 N 0.33869(19) 0.1683(3) 0.1481(2) 0.0677(6) Uani 1 1 d . . . N2 N 0.3967(2) 0.0638(4) 0.2191(2) 0.0863(8) Uani 1 1 d . . . N3 N 0.3315(3) -0.0542(4) 0.2291(3) 0.0868(8) Uani 1 1 d . . . N4 N 0.2310(2) -0.0327(3) 0.1655(2) 0.0696(7) Uani 1 1 d . . . C1 C -0.1429(3) 0.3395(3) 0.0544(3) 0.0738(8) Uani 1 1 d . . . H1A H -0.1854 0.3219 -0.0182 0.089 Uiso 1 1 calc R . . H1B H -0.0775 0.4016 0.0448 0.089 Uiso 1 1 calc R . . H1C H -0.1882 0.3957 0.1027 0.089 Uiso 1 1 calc R . . C2 C -0.0221(3) 0.2002(5) 0.2521(2) 0.0812(9) Uani 1 1 d . . . H2A H 0.0033 0.1043 0.2910 0.097 Uiso 1 1 calc R . . H2B H -0.0692 0.2587 0.2973 0.097 Uiso 1 1 calc R . . H2C H 0.0414 0.2644 0.2393 0.097 Uiso 1 1 calc R . . C3 C -0.2284(3) 0.0681(4) 0.1607(3) 0.0862(10) Uani 1 1 d . . . H3A H -0.2780 0.0388 0.0946 0.103 Uiso 1 1 calc R . . H3B H -0.2641 0.1465 0.2031 0.103 Uiso 1 1 calc R . . H3C H -0.2111 -0.0245 0.2070 0.103 Uiso 1 1 calc R . . C4 C 0.2369(2) 0.1070(3) 0.1143(2) 0.0536(6) Uani 1 1 d . . . C5 C 0.3902(3) 0.3139(4) 0.1102(3) 0.0855(10) Uani 1 1 d . . . H5A H 0.4483 0.3494 0.1685 0.103 Uiso 1 1 calc R . . H5B H 0.3340 0.3972 0.0989 0.103 Uiso 1 1 calc R . . C6 C 0.4398(4) 0.2880(7) 0.0030(5) 0.1252(18) Uani 1 1 d . . . H6 H 0.3863 0.2965 -0.0600 0.150 Uiso 1 1 calc R . . C7 C 0.5201(8) 0.2624(13) -0.0203(7) 0.259(6) Uani 1 1 d . . . H7A H 0.5809 0.2510 0.0352 0.311 Uiso 1 1 calc R . . H7B H 0.5300 0.2512 -0.0964 0.311 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 0.04514(18) 0.04265(18) 0.04649(18) -0.00427(9) 0.00191(11) -0.00199(9) P1 0.0599(4) 0.0506(4) 0.0526(3) -0.0058(3) 0.0086(3) 0.0036(3) S1 0.0558(4) 0.0491(4) 0.0689(4) 0.0020(3) -0.0025(3) -0.0079(3) N1 0.0584(13) 0.0769(16) 0.0648(13) 0.0037(12) -0.0053(10) -0.0168(11) N2 0.0701(16) 0.107(2) 0.0764(17) 0.0165(17) -0.0145(13) -0.0075(17) N3 0.0818(19) 0.097(2) 0.0776(18) 0.0284(17) -0.0073(15) -0.0067(17) N4 0.0703(16) 0.0709(15) 0.0660(15) 0.0166(12) 0.0019(12) -0.0131(13) C1 0.091(2) 0.0562(16) 0.0754(18) 0.0019(14) 0.0142(16) 0.0163(15) C2 0.094(2) 0.091(2) 0.0571(16) -0.0175(15) 0.0007(15) 0.0173(19) C3 0.083(2) 0.079(2) 0.105(3) -0.010(2) 0.043(2) -0.0030(18) C4 0.0529(13) 0.0588(14) 0.0487(12) -0.0016(11) 0.0045(10) -0.0088(11) C5 0.0706(19) 0.079(2) 0.104(3) 0.0020(19) -0.0009(18) -0.0275(17) C6 0.112(4) 0.147(5) 0.119(4) 0.015(3) 0.024(3) -0.056(3) C7 0.286(11) 0.362(13) 0.145(6) 0.070(8) 0.084(7) 0.210(11) _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 P1 2.3237(7) . ? Pd1 P1 2.3237(7) 3 ? Pd1 S1 2.3415(7) 3 ? Pd1 S1 2.3415(7) . ? P1 C2 1.803(3) . ? P1 C1 1.808(3) . ? P1 C3 1.810(3) . ? S1 C4 1.717(3) . ? N1 C4 1.343(3) . ? N1 N2 1.352(4) . ? N1 C5 1.464(4) . ? N2 N3 1.276(4) . ? N3 N4 1.359(4) . ? N4 C4 1.326(4) . ? C5 C6 1.484(6) . ? C6 C7 1.057(8) . ? 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 P1 Pd1 P1 180.00(3) . 3 ? P1 Pd1 S1 92.68(3) . 3 ? P1 Pd1 S1 87.32(3) 3 3 ? P1 Pd1 S1 87.32(3) . . ? P1 Pd1 S1 92.68(3) 3 . ? S1 Pd1 S1 180.0 3 . ? C2 P1 C1 104.80(17) . . ? C2 P1 C3 102.33(19) . . ? C1 P1 C3 104.13(17) . . ? C2 P1 Pd1 113.88(11) . . ? C1 P1 Pd1 111.41(11) . . ? C3 P1 Pd1 118.85(12) . . ? C4 S1 Pd1 100.14(9) . . ? C4 N1 N2 108.8(2) . . ? C4 N1 C5 129.1(3) . . ? N2 N1 C5 121.8(2) . . ? N3 N2 N1 106.5(3) . . ? N2 N3 N4 111.1(3) . . ? C4 N4 N3 106.3(2) . . ? N4 C4 N1 107.3(2) . . ? N4 C4 S1 128.5(2) . . ? N1 C4 S1 124.2(2) . . ? N1 C5 C6 111.6(3) . . ? C7 C6 C5 136.5(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.487 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.054 #=================================================================END data_abspd _database_code_CSD 210416 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H28 N8 P2 Pd S2' _chemical_formula_weight 612.96 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' S S 0.1246 0.1234 '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 'P2(1)/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 6.1906(14) _cell_length_b 17.205(3) _cell_length_c 12.664(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.531(15) _cell_angle_gamma 90.00 _cell_volume 1326.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 7.30 _cell_measurement_theta_max 12.55 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 1.003 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4630 _exptl_absorpt_correction_T_max 0.4770 _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 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2545 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2320 _reflns_number_gt 2032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0222P)^2^+0.9816P] 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 2320 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.0000 0.0000 0.5000 0.03171(10) Uani 1 2 d S . . S1 S 0.15170(14) -0.01511(4) 0.68077(6) 0.04803(19) Uani 1 1 d . . . P1 P 0.16872(12) -0.11118(4) 0.44738(6) 0.03988(17) Uani 1 1 d . . . N1 N -0.1214(4) -0.14169(15) 0.6675(2) 0.0531(6) Uani 1 1 d . . . N2 N -0.1359(5) -0.20618(17) 0.7282(3) 0.0651(8) Uani 1 1 d . . . N3 N 0.0180(5) -0.20772(15) 0.8117(2) 0.0605(7) Uani 1 1 d . . . N4 N 0.1410(4) -0.14264(13) 0.80702(19) 0.0443(6) Uani 1 1 d . . . C1 C 0.3206(6) -0.1770(2) 0.5450(3) 0.0745(11) Uani 1 1 d . . . H1A H 0.2267 -0.1954 0.5922 0.089 Uiso 1 1 calc R . . H1B H 0.4441 -0.1503 0.5861 0.089 Uiso 1 1 calc R . . H1C H 0.3715 -0.2204 0.5086 0.089 Uiso 1 1 calc R . . C2 C -0.0178(6) -0.17569(18) 0.3642(3) 0.0696(10) Uani 1 1 d . . . H2A H -0.1314 -0.1915 0.4020 0.083 Uiso 1 1 calc R . . H2B H 0.0608 -0.2206 0.3468 0.083 Uiso 1 1 calc R . . H2C H -0.0824 -0.1494 0.2992 0.083 Uiso 1 1 calc R . . C3 C 0.3739(8) -0.0850(2) 0.3699(4) 0.0941(15) Uani 1 1 d . . . H3A H 0.4784 -0.0504 0.4110 0.113 Uiso 1 1 calc R . . H3B H 0.3049 -0.0597 0.3049 0.113 Uiso 1 1 calc R . . H3C H 0.4479 -0.1310 0.3526 0.113 Uiso 1 1 calc R . . C4 C 0.0524(5) -0.10245(16) 0.7173(2) 0.0409(6) Uani 1 1 d . . . C5 C 0.3277(5) -0.12621(16) 0.8897(2) 0.0468(7) Uani 1 1 d . . . C6 C 0.3129(7) -0.1415(2) 0.9960(3) 0.0679(10) Uani 1 1 d . . . H10 H 0.1852 -0.1617 1.0140 0.081 Uiso 1 1 calc R . . C7 C 0.4962(9) -0.1253(3) 1.0745(3) 0.0851(14) Uani 1 1 d . . . H9 H 0.4912 -0.1357 1.1461 0.102 Uiso 1 1 calc R . . C8 C 0.6850(8) -0.0941(3) 1.0484(3) 0.0831(13) Uani 1 1 d . . . H8 H 0.8047 -0.0829 1.1021 0.100 Uiso 1 1 calc R . . C9 C 0.6953(6) -0.0799(2) 0.9444(3) 0.0679(10) Uani 1 1 d . . . H7 H 0.8224 -0.0586 0.9270 0.082 Uiso 1 1 calc R . . C10 C 0.5184(6) -0.09670(19) 0.8636(3) 0.0560(8) Uani 1 1 d . . . H6 H 0.5282 -0.0881 0.7921 0.067 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 0.03469(16) 0.02855(15) 0.03210(16) 0.00225(10) 0.00663(11) -0.00133(11) S1 0.0654(5) 0.0386(4) 0.0356(4) 0.0061(3) -0.0024(3) -0.0096(3) P1 0.0392(4) 0.0333(4) 0.0487(4) -0.0045(3) 0.0120(3) -0.0014(3) N1 0.0477(15) 0.0504(15) 0.0618(16) 0.0055(12) 0.0111(13) -0.0075(12) N2 0.0625(18) 0.0531(16) 0.083(2) 0.0102(15) 0.0226(17) -0.0118(14) N3 0.0717(19) 0.0462(15) 0.0677(18) 0.0130(13) 0.0231(16) -0.0066(14) N4 0.0518(14) 0.0372(12) 0.0459(13) 0.0079(10) 0.0140(11) 0.0032(11) C1 0.078(3) 0.066(2) 0.076(2) -0.0042(19) 0.006(2) 0.037(2) C2 0.068(2) 0.0377(17) 0.094(3) -0.0139(17) -0.007(2) -0.0024(16) C3 0.100(3) 0.069(3) 0.136(4) -0.012(3) 0.083(3) -0.011(2) C4 0.0470(16) 0.0364(14) 0.0408(14) 0.0033(11) 0.0124(12) 0.0018(12) C5 0.065(2) 0.0348(14) 0.0404(15) 0.0040(12) 0.0106(14) 0.0154(14) C6 0.101(3) 0.059(2) 0.0466(19) 0.0077(15) 0.0209(19) 0.016(2) C7 0.133(4) 0.082(3) 0.0353(17) 0.0014(18) 0.004(2) 0.036(3) C8 0.102(3) 0.079(3) 0.058(2) -0.014(2) -0.014(2) 0.022(3) C9 0.062(2) 0.066(2) 0.070(2) -0.0050(18) -0.0035(18) 0.0116(18) C10 0.063(2) 0.0559(19) 0.0473(17) 0.0033(15) 0.0058(15) 0.0120(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 S1 2.3248(8) 3_556 ? Pd1 S1 2.3248(8) . ? Pd1 P1 2.3341(8) . ? Pd1 P1 2.3341(8) 3_556 ? S1 C4 1.719(3) . ? P1 C2 1.797(3) . ? P1 C3 1.798(4) . ? P1 C1 1.809(3) . ? N1 C4 1.328(4) . ? N1 N2 1.362(4) . ? N2 N3 1.288(4) . ? N3 N4 1.361(3) . ? N4 C4 1.357(4) . ? N4 C5 1.439(4) . ? C5 C10 1.379(5) . ? C5 C6 1.390(4) . ? C6 C7 1.394(6) . ? C7 C8 1.380(6) . ? C8 C9 1.352(5) . ? C9 C10 1.387(5) . ? 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 S1 Pd1 S1 180.0 3_556 . ? S1 Pd1 P1 86.09(3) 3_556 . ? S1 Pd1 P1 93.91(3) . . ? S1 Pd1 P1 93.91(3) 3_556 3_556 ? S1 Pd1 P1 86.09(3) . 3_556 ? P1 Pd1 P1 180.00(3) . 3_556 ? C4 S1 Pd1 105.25(10) . . ? C2 P1 C3 106.1(2) . . ? C2 P1 C1 102.23(18) . . ? C3 P1 C1 101.5(2) . . ? C2 P1 Pd1 113.61(12) . . ? C3 P1 Pd1 110.38(14) . . ? C1 P1 Pd1 121.47(12) . . ? C4 N1 N2 106.1(3) . . ? N3 N2 N1 111.4(3) . . ? N2 N3 N4 106.4(2) . . ? C4 N4 N3 108.2(2) . . ? C4 N4 C5 131.1(2) . . ? N3 N4 C5 120.7(2) . . ? N1 C4 N4 107.9(2) . . ? N1 C4 S1 128.0(2) . . ? N4 C4 S1 124.1(2) . . ? C10 C5 C6 120.8(3) . . ? C10 C5 N4 120.4(3) . . ? C6 C5 N4 118.7(3) . . ? C5 C6 C7 117.7(4) . . ? C8 C7 C6 121.4(4) . . ? C9 C8 C7 119.8(4) . . ? C8 C9 C10 120.7(4) . . ? C5 C10 C9 119.6(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.282 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.057 #==============================================================END data_ncset _database_code_CSD 210417 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 N8 P2 Pt S2' _chemical_formula_weight 605.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 11.367(2) _cell_length_b 8.5306(11) _cell_length_c 11.5869(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.634(12) _cell_angle_gamma 90.00 _cell_volume 1121.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 5.06 _cell_measurement_theta_max 12.54 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 6.599 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5727 _exptl_absorpt_correction_T_max 0.8699 _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 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2066 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1963 _reflns_number_gt 1558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0179P)^2^+0.4143P] 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 1963 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0600 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Pt1 Pt 0.0000 0.0000 0.0000 0.03224(9) Uani 1 2 d S . . S1 S 0.14837(12) 0.18996(15) 0.01330(11) 0.0446(3) Uani 1 1 d . . . P1 P -0.10422(12) 0.15493(16) 0.12170(11) 0.0416(3) Uani 1 1 d . . . N1 N 0.2461(4) -0.0301(5) 0.1642(4) 0.0560(13) Uani 1 1 d . . . N2 N 0.3513(5) -0.0472(7) 0.2232(5) 0.0749(17) Uani 1 1 d . . . N3 N 0.4223(5) 0.0665(8) 0.2049(5) 0.0698(15) Uani 1 1 d . . . N4 N 0.3604(4) 0.1638(6) 0.1311(4) 0.0525(11) Uani 1 1 d . . . C1 C -0.2382(6) 0.0774(8) 0.1759(6) 0.0710(18) Uani 1 1 d . . . H1A H -0.2218 -0.0214 0.2132 0.085 Uiso 1 1 calc R . . H1B H -0.2960 0.0629 0.1128 0.085 Uiso 1 1 calc R . . H1C H -0.2679 0.1497 0.2306 0.085 Uiso 1 1 calc R . . C2 C -0.0208(5) 0.2087(8) 0.2540(4) 0.0671(18) Uani 1 1 d . . . H2A H 0.0063 0.1156 0.2939 0.081 Uiso 1 1 calc R . . H2B H -0.0701 0.2678 0.3023 0.081 Uiso 1 1 calc R . . H2C H 0.0458 0.2713 0.2358 0.081 Uiso 1 1 calc R . . C3 C -0.1498(6) 0.3387(7) 0.0551(5) 0.0624(16) Uani 1 1 d . . . H3A H -0.1951 0.3183 -0.0161 0.075 Uiso 1 1 calc R . . H3B H -0.0814 0.3993 0.0396 0.075 Uiso 1 1 calc R . . H3C H -0.1971 0.3959 0.1064 0.075 Uiso 1 1 calc R . . C4 C 0.2529(4) 0.1034(6) 0.1057(4) 0.0409(11) Uani 1 1 d . . . C5 C 0.4156(6) 0.3034(8) 0.0846(6) 0.0726(19) Uani 1 1 d . . . H5A H 0.4721 0.3462 0.1425 0.087 Uiso 1 1 calc R . . H5B H 0.3558 0.3824 0.0668 0.087 Uiso 1 1 calc R . . C6 C 0.4756(8) 0.2658(12) -0.0202(7) 0.113(3) Uani 1 1 d . . . H6A H 0.5107 0.3590 -0.0492 0.136 Uiso 1 1 calc R . . H6B H 0.4196 0.2244 -0.0778 0.136 Uiso 1 1 calc R . . H6C H 0.5360 0.1892 -0.0023 0.136 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02996(14) 0.03370(13) 0.03238(13) -0.00312(12) -0.00344(9) -0.00154(13) S1 0.0415(7) 0.0393(6) 0.0518(7) 0.0035(6) -0.0082(6) -0.0069(6) P1 0.0430(7) 0.0419(7) 0.0398(6) -0.0063(6) 0.0015(5) 0.0024(6) N1 0.050(3) 0.057(3) 0.060(3) 0.020(2) -0.006(2) -0.008(2) N2 0.061(4) 0.088(4) 0.073(4) 0.034(3) -0.017(3) -0.012(3) N3 0.052(3) 0.088(4) 0.067(3) 0.020(3) -0.017(3) -0.009(3) N4 0.039(2) 0.062(3) 0.054(3) 0.008(2) -0.014(2) -0.012(2) C1 0.066(4) 0.064(4) 0.086(5) -0.014(4) 0.032(4) -0.006(4) C2 0.073(5) 0.083(5) 0.044(3) -0.017(3) -0.009(3) 0.008(4) C3 0.083(4) 0.052(3) 0.053(3) -0.001(3) 0.013(3) 0.020(3) C4 0.036(2) 0.048(3) 0.039(2) -0.001(2) -0.002(2) -0.012(2) C5 0.054(4) 0.069(4) 0.093(5) 0.004(4) -0.007(3) -0.029(3) C6 0.120(8) 0.118(8) 0.105(7) 0.033(5) 0.040(6) -0.032(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 Pt1 P1 2.3131(13) 3 ? Pt1 P1 2.3131(13) . ? Pt1 S1 2.3369(13) . ? Pt1 S1 2.3369(13) 3 ? S1 C4 1.715(5) . ? P1 C3 1.808(6) . ? P1 C1 1.809(6) . ? P1 C2 1.809(5) . ? N1 C4 1.330(6) . ? N1 N2 1.347(7) . ? N2 N3 1.288(8) . ? N3 N4 1.356(7) . ? N4 C4 1.342(6) . ? N4 C5 1.465(7) . ? C5 C6 1.466(9) . ? 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 P1 Pt1 P1 180.00(6) 3 . ? P1 Pt1 S1 92.35(5) 3 . ? P1 Pt1 S1 87.65(5) . . ? P1 Pt1 S1 87.65(5) 3 3 ? P1 Pt1 S1 92.35(5) . 3 ? S1 Pt1 S1 180.0 . 3 ? C4 S1 Pt1 102.19(17) . . ? C3 P1 C1 103.9(3) . . ? C3 P1 C2 105.2(3) . . ? C1 P1 C2 101.9(3) . . ? C3 P1 Pt1 112.27(18) . . ? C1 P1 Pt1 118.6(2) . . ? C2 P1 Pt1 113.6(2) . . ? C4 N1 N2 105.8(4) . . ? N3 N2 N1 112.4(5) . . ? N2 N3 N4 105.0(5) . . ? C4 N4 N3 109.4(5) . . ? C4 N4 C5 129.6(5) . . ? N3 N4 C5 120.8(5) . . ? N1 C4 N4 107.4(5) . . ? N1 C4 S1 128.8(4) . . ? N4 C4 S1 123.9(4) . . ? N4 C5 C6 111.1(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.440 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.097 #============================================================END data_ptdepe _database_code_CSD 210418 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H46 N8 O2 P2 Pt S2' _chemical_formula_weight 847.88 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C222(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.155(3) _cell_length_b 19.510(5) _cell_length_c 15.766(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3738.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 3.63 _cell_measurement_theta_max 12.42 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 3.986 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4370 _exptl_absorpt_correction_T_max 0.8131 _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 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1825 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1825 _reflns_number_gt 1682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0700P)^2^+1.2678P] 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 0.002(19) _refine_ls_number_reflns 1825 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 Pt1 Pt 0.0000 -0.030224(18) -0.2500 0.03788(17) Uani 1 2 d S . . S1 S -0.0926(3) 0.05370(15) -0.16870(16) 0.0571(7) Uani 1 1 d . . . P1 P -0.0796(3) -0.11383(16) -0.1760(2) 0.0600(8) Uani 1 1 d . . . N1 N -0.2348(8) 0.1475(5) -0.2253(5) 0.049(2) Uani 1 1 d . . . N2 N -0.2891(10) 0.1667(6) -0.2962(7) 0.060(3) Uani 1 1 d . . . N3 N -0.2611(9) 0.1254(6) -0.3535(7) 0.062(3) Uani 1 1 d . . . N4 N -0.1871(9) 0.0781(5) -0.3234(6) 0.059(2) Uani 1 1 d . . . C1 C -0.1751(7) 0.0936(4) -0.2443(9) 0.0454(19) Uani 1 1 d . . . C2 C -0.2616(10) 0.1791(5) -0.1447(8) 0.050(3) Uani 1 1 d . . . C3 C -0.1906(11) 0.2298(6) -0.1127(8) 0.059(3) Uani 1 1 d . . . C4 C -0.2191(15) 0.2595(8) -0.0367(10) 0.067(4) Uani 1 1 d . . . H4 H -0.1732 0.2928 -0.0138 0.080 Uiso 1 1 calc R . . C5 C -0.3111(15) 0.2420(9) 0.0056(11) 0.077(5) Uani 1 1 d . . . H5 H -0.3292 0.2646 0.0556 0.092 Uiso 1 1 calc R . . C6 C -0.3791(13) 0.1907(7) -0.0250(8) 0.075(4) Uani 1 1 d . . . H6 H -0.4410 0.1778 0.0058 0.090 Uiso 1 1 calc R . . C7 C -0.3550(10) 0.1579(5) -0.1026(8) 0.056(3) Uani 1 1 d . . . C8 C -0.0879(13) 0.2493(7) -0.1624(11) 0.081(4) Uani 1 1 d . . . H8A H -0.0488 0.2846 -0.1325 0.122 Uiso 1 1 calc R . . H8B H -0.1087 0.2658 -0.2174 0.122 Uiso 1 1 calc R . . H8C H -0.0414 0.2098 -0.1685 0.122 Uiso 1 1 calc R . . C9 C -0.4253(14) 0.0949(11) -0.1359(10) 0.110(6) Uani 1 1 d . . . H9A H -0.3949 0.0787 -0.1884 0.165 Uiso 1 1 calc R . . H9B H -0.5000 0.1092 -0.1447 0.165 Uiso 1 1 calc R . . H9C H -0.4234 0.0587 -0.0946 0.165 Uiso 1 1 calc R . . C10 C -0.016(2) -0.1952(5) -0.2033(9) 0.084(5) Uani 1 1 d . . . H10A H 0.0489 -0.2023 -0.1686 0.101 Uiso 1 1 calc R . . H10B H -0.0671 -0.2323 -0.1922 0.101 Uiso 1 1 calc R . . C11 C -0.0653(15) -0.1030(10) -0.0581(9) 0.082(5) Uani 1 1 d . . . H11A H -0.1100 -0.0647 -0.0394 0.098 Uiso 1 1 calc R . . H11B H -0.0915 -0.1440 -0.0296 0.098 Uiso 1 1 calc R . . C12 C 0.050(2) -0.0908(13) -0.0352(15) 0.118(5) Uani 1 1 d . . . H12A H 0.0558 -0.0851 0.0251 0.177 Uiso 1 1 calc R . . H12B H 0.0756 -0.0501 -0.0631 0.177 Uiso 1 1 calc R . . H12C H 0.0938 -0.1292 -0.0527 0.177 Uiso 1 1 calc R . . C13 C -0.2234(15) -0.1348(10) -0.2013(17) 0.114(7) Uani 1 1 d . . . H13A H -0.2254 -0.1530 -0.2586 0.136 Uiso 1 1 calc R . . H13B H -0.2466 -0.1713 -0.1636 0.136 Uiso 1 1 calc R . . C14 C -0.3032(19) -0.0808(10) -0.1960(16) 0.118(5) Uani 1 1 d . . . H14A H -0.3742 -0.0982 -0.2118 0.177 Uiso 1 1 calc R . . H14B H -0.2828 -0.0443 -0.2336 0.177 Uiso 1 1 calc R . . H14C H -0.3061 -0.0638 -0.1389 0.177 Uiso 1 1 calc R . . O1 O -0.6019(7) -0.0489(3) -0.0672(4) 0.0507(17) 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 Pt1 0.0456(3) 0.0298(2) 0.0382(2) 0.000 -0.0026(4) 0.000 S1 0.0730(18) 0.0583(14) 0.0401(12) -0.0072(12) -0.0068(13) 0.0264(15) P1 0.0638(18) 0.0519(15) 0.0644(17) 0.0202(15) -0.0073(16) -0.0157(14) N1 0.053(5) 0.053(5) 0.040(6) 0.000(4) -0.005(4) 0.008(4) N2 0.070(7) 0.070(7) 0.039(5) 0.001(5) -0.009(5) 0.012(6) N3 0.068(6) 0.063(6) 0.056(6) 0.006(5) -0.001(5) 0.011(5) N4 0.070(6) 0.060(6) 0.047(5) -0.005(5) -0.009(5) 0.012(5) C1 0.054(4) 0.037(4) 0.046(5) -0.003(8) -0.008(7) 0.008(4) C2 0.055(6) 0.044(6) 0.051(7) 0.000(5) -0.003(5) 0.016(5) C3 0.069(8) 0.045(6) 0.064(7) -0.004(5) -0.010(6) 0.017(6) C4 0.080(10) 0.046(6) 0.073(9) -0.021(7) -0.021(8) 0.019(7) C5 0.094(13) 0.081(10) 0.054(8) -0.008(7) -0.007(9) 0.022(9) C6 0.087(10) 0.081(9) 0.057(7) 0.005(7) 0.021(7) 0.022(8) C7 0.062(7) 0.041(5) 0.064(7) -0.002(5) 0.009(6) 0.000(5) C8 0.087(10) 0.064(8) 0.093(10) -0.001(7) 0.005(9) -0.009(7) C9 0.091(11) 0.178(17) 0.061(7) -0.011(11) -0.005(8) -0.046(13) C10 0.127(16) 0.043(5) 0.084(7) -0.001(5) -0.026(12) -0.012(9) C11 0.101(12) 0.077(10) 0.068(8) 0.030(8) 0.024(8) 0.001(9) C12 0.128(11) 0.098(9) 0.129(12) 0.000(9) -0.015(11) 0.003(9) C13 0.093(12) 0.088(12) 0.160(19) 0.011(12) 0.010(13) -0.036(10) C14 0.128(11) 0.098(9) 0.129(12) 0.000(9) -0.015(11) 0.003(9) O1 0.080(5) 0.022(3) 0.050(4) 0.005(3) 0.001(4) 0.000(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 Pt1 P1 2.227(3) . ? Pt1 P1 2.227(3) 3_554 ? Pt1 S1 2.365(3) . ? Pt1 S1 2.365(3) 3_554 ? S1 C1 1.741(12) . ? P1 C10 1.817(16) . ? P1 C13 1.839(18) . ? P1 C11 1.879(15) . ? N1 C1 1.312(13) . ? N1 N2 1.352(13) . ? N1 C2 1.450(15) . ? N2 N3 1.257(15) . ? N3 N4 1.374(14) . ? N4 C1 1.292(17) . ? C2 C7 1.379(16) . ? C2 C3 1.406(17) . ? C3 C4 1.375(19) . ? C3 C8 1.52(2) . ? C4 C5 1.35(2) . ? C5 C6 1.38(2) . ? C6 C7 1.412(17) . ? C7 C9 1.586(19) . ? C10 C10 1.52(3) 3_554 ? C11 C12 1.47(2) . ? C13 C14 1.43(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 P1 Pt1 P1 85.80(19) . 3_554 ? P1 Pt1 S1 90.93(12) . . ? P1 Pt1 S1 176.53(13) 3_554 . ? P1 Pt1 S1 176.53(13) . 3_554 ? P1 Pt1 S1 90.93(12) 3_554 3_554 ? S1 Pt1 S1 92.36(16) . 3_554 ? C1 S1 Pt1 102.3(4) . . ? C10 P1 C13 99.1(10) . . ? C10 P1 C11 107.0(7) . . ? C13 P1 C11 109.1(10) . . ? C10 P1 Pt1 109.3(6) . . ? C13 P1 Pt1 117.5(7) . . ? C11 P1 Pt1 113.3(5) . . ? C1 N1 N2 107.7(9) . . ? C1 N1 C2 131.7(10) . . ? N2 N1 C2 119.8(9) . . ? N3 N2 N1 106.5(9) . . ? N2 N3 N4 111.2(10) . . ? C1 N4 N3 104.4(9) . . ? N4 C1 N1 110.2(10) . . ? N4 C1 S1 128.4(8) . . ? N1 C1 S1 121.3(10) . . ? C7 C2 C3 122.9(11) . . ? C7 C2 N1 118.7(11) . . ? C3 C2 N1 118.5(11) . . ? C4 C3 C2 117.1(13) . . ? C4 C3 C8 123.3(13) . . ? C2 C3 C8 119.6(11) . . ? C5 C4 C3 122.3(14) . . ? C4 C5 C6 120.5(14) . . ? C5 C6 C7 120.3(14) . . ? C2 C7 C6 117.0(12) . . ? C2 C7 C9 121.1(11) . . ? C6 C7 C9 121.7(12) . . ? C10 C10 P1 109.7(8) 3_554 . ? C12 C11 P1 110.5(13) . . ? C14 C13 P1 117.8(14) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.604 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.135 #==============================================================END data_2s-or _database_code_CSD 210419 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 N4 O S' _chemical_formula_weight 310.37 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' S S 0.1246 0.1234 '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 7.956(3) _cell_length_b 9.962(3) _cell_length_c 11.165(3) _cell_angle_alpha 91.151(18) _cell_angle_beta 107.51(2) _cell_angle_gamma 111.21(2) _cell_volume 778.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 4.69 _cell_measurement_theta_max 12.52 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'COLORLESS ' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 324 _exptl_absorpt_coefficient_mu 0.215 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5739 _exptl_absorpt_correction_T_max 0.8704 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2905 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2697 _reflns_number_gt 1440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.1248P)^2^+1.6783P] 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 2697 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1703 _refine_ls_R_factor_gt 0.0995 _refine_ls_wR_factor_ref 0.3026 _refine_ls_wR_factor_gt 0.2505 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 S1 S 0.3719(3) 0.3221(2) 0.4279(2) 0.0816(8) Uani 1 1 d . . . O1 O 0.0883(8) 0.1282(6) 0.2830(4) 0.0788(18) Uani 1 1 d . . . N1 N 0.2588(7) 0.4201(5) 0.1964(5) 0.0490(12) Uani 1 1 d . . . N2 N 0.1868(9) 0.5187(7) 0.1560(7) 0.0752(18) Uani 1 1 d . . . N3 N 0.1281(9) 0.5521(6) 0.2444(7) 0.0773(18) Uani 1 1 d . . . N4 N 0.1606(10) 0.4828(8) 0.3408(6) 0.0799(19) Uani 1 1 d . . . C1 C 0.3388(9) 0.3556(6) 0.1197(6) 0.0487(15) Uani 1 1 d . . . C2 C 0.5371(8) 0.4101(7) 0.1519(6) 0.0495(15) Uani 1 1 d . . . C3 C 0.6095(10) 0.3472(8) 0.0790(6) 0.0614(17) Uani 1 1 d . . . H3 H 0.7408 0.3813 0.0959 0.074 Uiso 1 1 calc R . . C4 C 0.4918(12) 0.2361(9) -0.0171(7) 0.073(2) Uani 1 1 d . . . H4 H 0.5447 0.1934 -0.0625 0.088 Uiso 1 1 calc R . . C5 C 0.2968(11) 0.1857(8) -0.0487(7) 0.0675(19) Uani 1 1 d . . . H5 H 0.2192 0.1113 -0.1162 0.081 Uiso 1 1 calc R . . C6 C 0.2154(9) 0.2457(7) 0.0202(6) 0.0576(17) Uani 1 1 d . . . C7 C 0.6693(9) 0.5339(7) 0.2590(6) 0.0650(19) Uani 1 1 d . . . H7A H 0.5948 0.5647 0.2985 0.098 Uiso 1 1 calc R . . H7B H 0.7424 0.6140 0.2256 0.098 Uiso 1 1 calc R . . H7C H 0.7541 0.5014 0.3206 0.098 Uiso 1 1 calc R . . C8 C -0.0017(9) 0.1950(8) -0.0164(7) 0.076(2) Uani 1 1 d . . . H8A H -0.0621 0.1185 -0.0874 0.114 Uiso 1 1 calc R . . H8B H -0.0386 0.2752 -0.0391 0.114 Uiso 1 1 calc R . . H8C H -0.0405 0.1596 0.0542 0.114 Uiso 1 1 calc R . . C9 C 0.2496(11) 0.4067(8) 0.3141(7) 0.071(2) Uani 1 1 d . . . C10 C 0.1970(14) 0.1381(8) 0.3735(11) 0.087(3) Uani 1 1 d . . . C11 C 0.2467(11) 0.0401(7) 0.4726(7) 0.0644(18) Uani 1 1 d . . . C12 C 0.3854(13) 0.0833(9) 0.5886(9) 0.083(2) Uani 1 1 d . . . H12 H 0.4633 0.1812 0.6155 0.100 Uiso 1 1 calc R . . C13 C 0.4101(13) -0.0213(10) 0.6676(7) 0.087(3) Uani 1 1 d . . . H13 H 0.5061 0.0067 0.7463 0.105 Uiso 1 1 calc R . . C14 C 0.2898(15) -0.1666(10) 0.6267(8) 0.088(3) Uani 1 1 d . . . H14 H 0.3033 -0.2365 0.6786 0.106 Uiso 1 1 calc R . . C15 C 0.1534(12) -0.2059(8) 0.5116(8) 0.080(2) Uani 1 1 d . . . H15 H 0.0742 -0.3035 0.4839 0.096 Uiso 1 1 calc R . . C16 C 0.1302(11) -0.1043(8) 0.4354(8) 0.076(2) Uani 1 1 d . . . H16 H 0.0338 -0.1334 0.3568 0.091 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 S1 0.0789(14) 0.0592(12) 0.0895(15) 0.0094(10) 0.0159(11) 0.0171(10) O1 0.083(4) 0.122(5) 0.040(3) 0.034(3) 0.005(2) 0.060(3) N1 0.045(3) 0.050(3) 0.057(3) 0.015(2) 0.018(2) 0.023(2) N2 0.088(4) 0.069(4) 0.100(5) 0.041(4) 0.047(4) 0.051(4) N3 0.067(4) 0.053(4) 0.118(6) 0.013(4) 0.038(4) 0.025(3) N4 0.092(5) 0.096(5) 0.084(5) 0.027(4) 0.042(4) 0.061(4) C1 0.053(4) 0.047(3) 0.049(3) 0.015(3) 0.018(3) 0.021(3) C2 0.047(4) 0.054(4) 0.055(4) 0.018(3) 0.022(3) 0.023(3) C3 0.058(4) 0.073(5) 0.054(4) 0.012(3) 0.019(3) 0.026(4) C4 0.084(6) 0.082(5) 0.067(5) 0.005(4) 0.033(4) 0.040(5) C5 0.079(5) 0.058(4) 0.056(4) 0.002(3) 0.018(4) 0.020(4) C6 0.057(4) 0.052(4) 0.060(4) 0.019(3) 0.011(3) 0.022(3) C7 0.051(4) 0.064(4) 0.067(4) -0.001(3) 0.015(3) 0.011(3) C8 0.055(4) 0.071(5) 0.075(5) 0.007(4) 0.004(4) 0.009(4) C9 0.089(5) 0.071(5) 0.074(5) 0.028(4) 0.037(4) 0.047(4) C10 0.097(7) 0.054(4) 0.141(9) 0.019(5) 0.073(7) 0.035(5) C11 0.074(5) 0.054(4) 0.078(5) 0.022(4) 0.034(4) 0.032(4) C12 0.100(6) 0.060(5) 0.101(6) 0.007(4) 0.035(5) 0.041(5) C13 0.094(6) 0.103(7) 0.062(5) -0.006(5) 0.007(4) 0.053(6) C14 0.133(8) 0.090(6) 0.078(6) 0.035(5) 0.044(6) 0.075(6) C15 0.097(6) 0.055(4) 0.091(6) 0.022(4) 0.037(5) 0.028(4) C16 0.076(5) 0.074(5) 0.076(5) 0.025(4) 0.025(4) 0.029(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 S1 C9 1.779(7) . ? S1 C10 1.807(9) . ? O1 C10 1.090(11) . ? N1 N2 1.329(7) . ? N1 C9 1.345(8) . ? N1 C1 1.467(7) . ? N2 N3 1.297(8) . ? N3 N4 1.301(9) . ? N4 C9 1.293(9) . ? C1 C6 1.384(9) . ? C1 C2 1.394(8) . ? C2 C3 1.382(9) . ? C2 C7 1.518(9) . ? C3 C4 1.360(10) . ? C4 C5 1.372(10) . ? C5 C6 1.389(9) . ? C6 C8 1.530(9) . ? C10 C11 1.546(12) . ? C11 C12 1.362(11) . ? C11 C16 1.372(10) . ? C12 C13 1.407(11) . ? C13 C14 1.389(12) . ? C14 C15 1.347(12) . ? C15 C16 1.364(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 C9 S1 C10 96.9(5) . . ? N2 N1 C9 106.1(5) . . ? N2 N1 C1 121.5(5) . . ? C9 N1 C1 132.3(5) . . ? N3 N2 N1 106.0(6) . . ? N2 N3 N4 112.5(6) . . ? C9 N4 N3 105.2(6) . . ? C6 C1 C2 123.7(6) . . ? C6 C1 N1 118.9(6) . . ? C2 C1 N1 117.4(5) . . ? C3 C2 C1 116.4(6) . . ? C3 C2 C7 120.8(6) . . ? C1 C2 C7 122.7(6) . . ? C4 C3 C2 121.1(7) . . ? C3 C4 C5 121.6(7) . . ? C4 C5 C6 120.0(7) . . ? C1 C6 C5 117.1(6) . . ? C1 C6 C8 122.0(6) . . ? C5 C6 C8 120.9(6) . . ? N4 C9 N1 110.0(6) . . ? N4 C9 S1 123.3(6) . . ? N1 C9 S1 126.0(5) . . ? O1 C10 C11 138.6(8) . . ? O1 C10 S1 112.5(7) . . ? C11 C10 S1 108.8(7) . . ? C12 C11 C16 119.5(7) . . ? C12 C11 C10 127.2(7) . . ? C16 C11 C10 113.3(7) . . ? C11 C12 C13 119.6(8) . . ? C14 C13 C12 119.3(8) . . ? C15 C14 C13 119.8(8) . . ? C14 C15 C16 120.7(8) . . ? C15 C16 C11 121.1(8) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.649 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.071 #================================================================END data_s2 _database_code_CSD 210420 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H18 N8 S2' _chemical_formula_weight 410.52 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 11.115(3) _cell_length_b 13.732(3) _cell_length_c 13.616(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.46(2) _cell_angle_gamma 90.00 _cell_volume 2074.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 5.35 _cell_measurement_theta_max 12.37 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'COLORLESS ' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5316 _exptl_absorpt_correction_T_max 0.8539 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3692 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.1120 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3494 _reflns_number_gt 1504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0750P)^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 0.0003(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3494 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1824 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.1955 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 S1 S 1.04762(14) 0.08469(11) 0.27732(13) 0.0677(5) Uani 1 1 d . . . S2 S 0.94053(13) 0.08558(12) 0.39254(12) 0.0628(5) Uani 1 1 d . . . N1 N 1.1004(4) 0.2389(3) 0.1658(4) 0.0566(13) Uani 1 1 d . . . N2 N 1.0678(5) 0.3342(3) 0.1473(4) 0.0790(17) Uani 1 1 d . . . N3 N 0.9865(5) 0.3541(4) 0.2085(5) 0.0846(18) Uani 1 1 d . . . N4 N 0.9601(5) 0.2750(4) 0.2658(4) 0.0767(16) Uani 1 1 d . . . N5 N 0.6982(4) 0.0794(3) 0.3806(4) 0.0615(13) Uani 1 1 d . . . N6 N 0.6025(5) 0.0683(4) 0.3140(5) 0.0803(17) Uani 1 1 d . . . N7 N 0.6482(6) 0.0569(4) 0.2294(5) 0.0886(19) Uani 1 1 d . . . N8 N 0.7711(5) 0.0588(4) 0.2371(4) 0.0708(15) Uani 1 1 d . . . C1 C 1.1842(5) 0.1875(4) 0.1091(5) 0.0555(15) Uani 1 1 d . . . C2 C 1.1370(6) 0.1375(4) 0.0263(5) 0.0669(17) Uani 1 1 d . . . C3 C 1.2181(8) 0.0881(5) -0.0278(5) 0.091(2) Uani 1 1 d . . . H3 H 1.1905 0.0532 -0.0832 0.109 Uiso 1 1 calc R . . C4 C 1.3403(8) 0.0896(6) -0.0006(7) 0.104(3) Uani 1 1 d . . . H4 H 1.3939 0.0570 -0.0389 0.125 Uiso 1 1 calc R . . C5 C 1.3832(6) 0.1387(6) 0.0824(7) 0.092(2) Uani 1 1 d . . . H5 H 1.4653 0.1377 0.1002 0.110 Uiso 1 1 calc R . . C6 C 1.3059(6) 0.1899(5) 0.1399(5) 0.0700(19) Uani 1 1 d . . . C7 C 1.0044(6) 0.1363(5) -0.0016(5) 0.092(2) Uani 1 1 d . . . H7A H 0.9627 0.1746 0.0446 0.138 Uiso 1 1 calc R . . H7B H 0.9753 0.0705 -0.0010 0.138 Uiso 1 1 calc R . . H7C H 0.9902 0.1632 -0.0664 0.138 Uiso 1 1 calc R . . C8 C 1.3507(6) 0.2470(6) 0.2295(5) 0.097(2) Uani 1 1 d . . . H8A H 1.4364 0.2392 0.2396 0.146 Uiso 1 1 calc R . . H8B H 1.3123 0.2234 0.2862 0.146 Uiso 1 1 calc R . . H8C H 1.3319 0.3147 0.2198 0.146 Uiso 1 1 calc R . . C9 C 1.0336(5) 0.2069(4) 0.2382(5) 0.0555(16) Uani 1 1 d . . . C10 C 0.6859(5) 0.0935(5) 0.4840(5) 0.0597(16) Uani 1 1 d . . . C11 C 0.6847(5) 0.1889(5) 0.5189(6) 0.0734(19) Uani 1 1 d . . . C12 C 0.6785(7) 0.2003(6) 0.6176(7) 0.099(3) Uani 1 1 d . . . H12 H 0.6808 0.2627 0.6441 0.118 Uiso 1 1 calc R . . C13 C 0.6689(7) 0.1209(8) 0.6799(6) 0.101(3) Uani 1 1 d . . . H13 H 0.6650 0.1303 0.7472 0.122 Uiso 1 1 calc R . . C14 C 0.6653(6) 0.0293(6) 0.6419(6) 0.081(2) Uani 1 1 d . . . H14 H 0.6552 -0.0230 0.6839 0.097 Uiso 1 1 calc R . . C15 C 0.6760(5) 0.0117(5) 0.5442(5) 0.0649(17) Uani 1 1 d . . . C16 C 0.6903(6) 0.2740(5) 0.4499(6) 0.102(3) Uani 1 1 d . . . H16A H 0.6952 0.2506 0.3838 0.153 Uiso 1 1 calc R . . H16B H 0.7602 0.3126 0.4679 0.153 Uiso 1 1 calc R . . H16C H 0.6191 0.3130 0.4538 0.153 Uiso 1 1 calc R . . C17 C 0.6724(6) -0.0892(5) 0.5011(5) 0.089(2) Uani 1 1 d . . . H17A H 0.6828 -0.0855 0.4317 0.133 Uiso 1 1 calc R . . H17B H 0.5961 -0.1188 0.5119 0.133 Uiso 1 1 calc R . . H17C H 0.7361 -0.1276 0.5322 0.133 Uiso 1 1 calc R . . C18 C 0.7982(5) 0.0726(4) 0.3305(5) 0.0541(15) 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 S1 0.0649(10) 0.0464(9) 0.0941(13) 0.0144(9) 0.0247(9) 0.0112(8) S2 0.0549(9) 0.0603(10) 0.0734(11) 0.0077(9) 0.0053(8) -0.0007(8) N1 0.055(3) 0.037(3) 0.079(4) 0.007(3) 0.010(3) -0.001(2) N2 0.082(4) 0.035(3) 0.122(5) 0.012(3) 0.021(4) 0.006(3) N3 0.083(4) 0.042(3) 0.131(6) 0.004(3) 0.024(4) 0.005(3) N4 0.071(4) 0.053(4) 0.108(5) -0.002(3) 0.016(3) 0.007(3) N5 0.053(3) 0.057(3) 0.074(4) 0.003(3) 0.000(3) -0.004(3) N6 0.061(4) 0.093(5) 0.086(4) 0.000(4) -0.003(3) -0.004(3) N7 0.081(5) 0.091(5) 0.092(5) 0.002(4) -0.015(4) -0.004(4) N8 0.078(4) 0.074(4) 0.060(4) -0.006(3) 0.004(3) -0.001(3) C1 0.056(4) 0.044(3) 0.068(4) 0.008(3) 0.015(3) 0.007(3) C2 0.075(5) 0.051(4) 0.075(5) 0.006(4) 0.013(4) -0.002(3) C3 0.108(6) 0.075(5) 0.092(6) -0.013(4) 0.027(5) -0.003(5) C4 0.092(7) 0.104(7) 0.120(8) -0.011(6) 0.039(6) 0.015(6) C5 0.054(4) 0.092(6) 0.131(7) 0.012(5) 0.017(5) 0.004(4) C6 0.057(4) 0.059(4) 0.094(5) 0.013(4) 0.006(4) -0.001(3) C7 0.087(5) 0.086(5) 0.101(6) -0.001(5) -0.017(4) -0.004(4) C8 0.081(5) 0.087(5) 0.122(7) 0.010(5) -0.010(5) -0.011(4) C9 0.045(3) 0.042(3) 0.081(5) 0.002(3) 0.010(3) 0.004(3) C10 0.053(4) 0.059(4) 0.068(4) -0.008(4) 0.011(3) 0.001(3) C11 0.054(4) 0.067(5) 0.099(6) -0.007(4) 0.002(4) 0.004(3) C12 0.079(5) 0.097(7) 0.119(8) -0.051(6) 0.000(5) 0.007(5) C13 0.084(5) 0.138(8) 0.083(6) -0.024(6) 0.010(5) 0.015(6) C14 0.061(4) 0.089(6) 0.094(6) 0.004(5) 0.023(4) 0.008(4) C15 0.054(4) 0.064(4) 0.078(5) 0.000(4) 0.006(3) -0.001(3) C16 0.082(5) 0.066(5) 0.156(8) -0.006(5) 0.001(5) 0.003(4) C17 0.100(6) 0.060(4) 0.108(6) 0.004(5) 0.021(5) -0.002(4) C18 0.047(3) 0.039(3) 0.076(5) -0.003(3) 0.005(3) -0.002(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 S1 C9 1.764(6) . ? S1 S2 2.026(2) . ? S2 C18 1.757(6) . ? N1 C9 1.343(7) . ? N1 N2 1.377(6) . ? N1 C1 1.431(7) . ? N2 N3 1.295(7) . ? N3 N4 1.379(7) . ? N4 C9 1.313(7) . ? N5 C18 1.342(7) . ? N5 N6 1.365(7) . ? N5 C10 1.436(7) . ? N6 N7 1.295(7) . ? N7 N8 1.365(7) . ? N8 C18 1.303(7) . ? C1 C6 1.393(8) . ? C1 C2 1.394(8) . ? C2 C3 1.377(9) . ? C2 C7 1.500(9) . ? C3 C4 1.387(10) . ? C4 C5 1.377(10) . ? C5 C6 1.389(9) . ? C6 C8 1.509(9) . ? C10 C11 1.394(8) . ? C10 C15 1.398(8) . ? C11 C12 1.358(10) . ? C11 C16 1.503(9) . ? C12 C13 1.390(11) . ? C13 C14 1.359(11) . ? C14 C15 1.365(9) . ? C15 C17 1.503(8) . ? 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 C9 S1 S2 100.6(2) . . ? C18 S2 S1 100.4(2) . . ? C9 N1 N2 107.1(5) . . ? C9 N1 C1 129.8(5) . . ? N2 N1 C1 122.9(5) . . ? N3 N2 N1 105.7(5) . . ? N2 N3 N4 112.2(5) . . ? C9 N4 N3 104.0(5) . . ? C18 N5 N6 106.9(5) . . ? C18 N5 C10 129.7(5) . . ? N6 N5 C10 123.4(5) . . ? N7 N6 N5 105.8(5) . . ? N6 N7 N8 112.0(5) . . ? C18 N8 N7 104.4(5) . . ? C6 C1 C2 124.5(6) . . ? C6 C1 N1 118.5(6) . . ? C2 C1 N1 117.0(6) . . ? C3 C2 C1 116.6(7) . . ? C3 C2 C7 121.6(7) . . ? C1 C2 C7 121.7(6) . . ? C2 C3 C4 120.8(8) . . ? C5 C4 C3 120.8(7) . . ? C4 C5 C6 121.1(7) . . ? C5 C6 C1 116.1(7) . . ? C5 C6 C8 122.3(7) . . ? C1 C6 C8 121.6(6) . . ? N4 C9 N1 111.0(5) . . ? N4 C9 S1 129.5(5) . . ? N1 C9 S1 119.4(4) . . ? C11 C10 C15 123.6(6) . . ? C11 C10 N5 117.6(6) . . ? C15 C10 N5 118.8(6) . . ? C12 C11 C10 116.5(7) . . ? C12 C11 C16 122.4(7) . . ? C10 C11 C16 121.1(7) . . ? C11 C12 C13 121.6(8) . . ? C14 C13 C12 119.7(8) . . ? C13 C14 C15 122.2(8) . . ? C14 C15 C10 116.3(6) . . ? C14 C15 C17 122.8(7) . . ? C10 C15 C17 120.9(6) . . ? N8 C18 N5 110.9(5) . . ? N8 C18 S2 129.2(5) . . ? N5 C18 S2 119.9(5) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.274 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.051