# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[Zn(LH2)2Br2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 Br2 N8 S2 Zn, 2(C H4 O)' _chemical_formula_sum 'C22 H28 Br2 N8 O2 S2 Zn' _chemical_formula_weight 725.83 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2989(11) _cell_length_b 12.4402(16) _cell_length_c 14.7088(19) _cell_angle_alpha 74.448(2) _cell_angle_beta 83.939(2) _cell_angle_gamma 85.086(2) _cell_volume 1452.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3275 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.10 _exptl_crystal_description BLOCK _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 3.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3688 _exptl_absorpt_correction_T_max 0.5497 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7763 _diffrn_reflns_av_R_equivalents 0.0141 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5109 _reflns_number_gt 4116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0471P)^2^+0.7157P] 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 5109 _refine_ls_number_parameters 362 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Br1 Br 1.08439(5) 0.61110(3) 0.84935(3) 0.05548(13) Uani 1 1 d . . . Br2 Br 1.04988(4) 0.28590(3) 0.86647(3) 0.05839(14) Uani 1 1 d . . . Zn1 Zn 0.92741(4) 0.47364(3) 0.82107(3) 0.04097(12) Uani 1 1 d . . . S1 S 0.91219(14) 0.49489(8) 0.65747(7) 0.0584(3) Uani 1 1 d . . . S2 S 0.66822(10) 0.49228(7) 0.89704(7) 0.0481(2) Uani 1 1 d . . . N1 N 0.7262(5) 1.0286(3) 0.4676(3) 0.0695(10) Uani 1 1 d D . . H1N H 0.709(6) 0.963(2) 0.466(3) 0.083 Uiso 1 1 d D . . N2 N 0.8433(4) 0.8234(2) 0.6042(2) 0.0529(8) Uani 1 1 d . . . N3 N 0.8862(4) 0.7124(2) 0.6455(2) 0.0529(8) Uani 1 1 d D . . H3N H 0.943(4) 0.694(3) 0.693(2) 0.064 Uiso 1 1 d D . . N4 N 0.7693(5) 0.6581(3) 0.5334(3) 0.0691(10) Uani 1 1 d D . . H4A H 0.731(6) 0.726(2) 0.513(3) 0.083 Uiso 1 1 d D . . H4B H 0.758(6) 0.612(3) 0.503(3) 0.083 Uiso 1 1 d D . . N5 N 0.2899(3) 0.0496(2) 0.8948(2) 0.0430(7) Uani 1 1 d D . . H5N H 0.301(4) 0.1159(19) 0.898(3) 0.052 Uiso 1 1 d D . . N6 N 0.5552(3) 0.1950(2) 0.88327(19) 0.0362(6) Uani 1 1 d . . . N7 N 0.6381(3) 0.2862(2) 0.8840(2) 0.0400(6) Uani 1 1 d D . . H7N H 0.739(2) 0.276(3) 0.887(2) 0.048 Uiso 1 1 d D . . N8 N 0.4026(3) 0.3904(2) 0.8997(2) 0.0476(7) Uani 1 1 d D . . H8A H 0.349(4) 0.334(2) 0.903(3) 0.057 Uiso 1 1 d D . . H8B H 0.355(4) 0.451(2) 0.905(3) 0.057 Uiso 1 1 d D . . C1 C 0.6684(7) 1.1190(4) 0.3983(4) 0.0906(16) Uani 1 1 d . . . H1 H 0.6175 1.1141 0.3463 0.109 Uiso 1 1 calc R . . C2 C 0.6974(7) 1.2145(4) 0.4180(4) 0.0885(16) Uani 1 1 d . . . H2 H 0.6706 1.2863 0.3819 0.106 Uiso 1 1 calc R . . C3 C 0.7758(6) 1.1875(3) 0.5031(3) 0.0666(12) Uani 1 1 d . . . C4 C 0.8352(6) 1.2487(4) 0.5571(4) 0.0766(14) Uani 1 1 d . . . H4 H 0.8233 1.3263 0.5398 0.092 Uiso 1 1 calc R . . C5 C 0.9113(7) 1.1939(4) 0.6359(4) 0.0790(14) Uani 1 1 d . . . H5 H 0.9517 1.2347 0.6721 0.095 Uiso 1 1 calc R . . C6 C 0.9291(6) 1.0774(3) 0.6627(3) 0.0702(12) Uani 1 1 d . . . H6 H 0.9823 1.0424 0.7164 0.084 Uiso 1 1 calc R . . C7 C 0.8703(5) 1.0117(3) 0.6122(3) 0.0527(9) Uani 1 1 d . . . C8 C 0.7927(5) 1.0683(3) 0.5319(3) 0.0565(10) Uani 1 1 d . . . C9 C 0.8956(5) 0.8915(3) 0.6440(3) 0.0547(10) Uani 1 1 d . . . H9 H 0.9537 0.8619 0.6967 0.066 Uiso 1 1 calc R . . C10 C 0.8499(5) 0.6319(3) 0.6092(3) 0.0508(9) Uani 1 1 d . . . C11 C 0.1543(4) -0.0088(3) 0.8997(3) 0.0520(9) Uani 1 1 d . . . H11 H 0.0478 0.0198 0.9066 0.062 Uiso 1 1 calc R . . C12 C 0.1979(4) -0.1129(3) 0.8931(3) 0.0515(9) Uani 1 1 d . . . H12 H 0.1284 -0.1682 0.8945 0.062 Uiso 1 1 calc R . . C13 C 0.3715(4) -0.1229(3) 0.8836(2) 0.0395(7) Uani 1 1 d . . . C14 C 0.4869(5) -0.2089(3) 0.8761(3) 0.0492(9) Uani 1 1 d . . . H14 H 0.4545 -0.2777 0.8736 0.059 Uiso 1 1 calc R . . C15 C 0.6497(5) -0.1911(3) 0.8722(3) 0.0544(10) Uani 1 1 d . . . H15 H 0.7270 -0.2487 0.8683 0.065 Uiso 1 1 calc R . . C16 C 0.6989(4) -0.0877(3) 0.8741(3) 0.0487(9) Uani 1 1 d . . . H16 H 0.8094 -0.0781 0.8716 0.058 Uiso 1 1 calc R . . C17 C 0.5899(4) 0.0019(2) 0.8797(2) 0.0363(7) Uani 1 1 d . . . C18 C 0.4245(4) -0.0189(3) 0.8859(2) 0.0357(7) Uani 1 1 d . . . C19 C 0.6478(4) 0.1075(3) 0.8807(2) 0.0403(8) Uani 1 1 d . . . H19 H 0.7592 0.1126 0.8794 0.048 Uiso 1 1 calc R . . C20 C 0.5614(4) 0.3822(2) 0.8927(2) 0.0349(7) Uani 1 1 d . . . O1 O 0.6018(5) 0.8436(4) 0.4214(3) 0.1020(12) Uani 1 1 d . . . H1A H 0.5112 0.8292 0.4480 0.153 Uiso 1 1 calc R . . C21 C 0.5981(11) 0.8584(7) 0.3309(4) 0.155(3) Uani 1 1 d . . . H21A H 0.5472 0.9306 0.3040 0.232 Uiso 1 1 calc R . . H21B H 0.5374 0.8016 0.3196 0.232 Uiso 1 1 calc R . . H21C H 0.7068 0.8539 0.3020 0.232 Uiso 1 1 calc R . . O2 O 0.6806(8) 0.5193(4) 0.4184(4) 0.154(2) Uani 1 1 d . . . H2A H 0.6386 0.4736 0.4638 0.232 Uiso 1 1 calc RD . . C22 C 0.5812(9) 0.5473(6) 0.3490(5) 0.120(2) Uani 1 1 d . . . H22A H 0.4715 0.5556 0.3755 0.180 Uiso 1 1 calc R . . H22B H 0.5893 0.4897 0.3161 0.180 Uiso 1 1 calc R . . H22C H 0.6111 0.6166 0.3056 0.180 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 Br1 0.0504(2) 0.0344(2) 0.0864(3) -0.01493(18) -0.02303(19) -0.01079(15) Br2 0.0313(2) 0.02932(19) 0.1131(3) -0.01318(19) -0.01588(19) 0.00050(14) Zn1 0.0323(2) 0.0263(2) 0.0648(3) -0.01123(17) -0.00589(17) -0.00493(15) S1 0.0791(7) 0.0362(5) 0.0636(6) -0.0179(4) -0.0106(5) -0.0038(5) S2 0.0353(5) 0.0327(4) 0.0827(6) -0.0270(4) 0.0033(4) -0.0086(3) N1 0.088(3) 0.049(2) 0.067(2) -0.0067(19) -0.016(2) 0.0013(19) N2 0.068(2) 0.0345(16) 0.0554(18) -0.0075(14) -0.0095(15) -0.0039(14) N3 0.069(2) 0.0333(16) 0.0563(19) -0.0075(14) -0.0182(16) -0.0014(14) N4 0.092(3) 0.048(2) 0.073(2) -0.0156(18) -0.031(2) -0.006(2) N5 0.0343(15) 0.0290(14) 0.0692(19) -0.0176(14) -0.0074(13) -0.0036(12) N6 0.0296(14) 0.0275(13) 0.0533(16) -0.0117(12) -0.0048(12) -0.0073(11) N7 0.0246(14) 0.0297(14) 0.0693(19) -0.0178(13) -0.0055(13) -0.0043(11) N8 0.0288(16) 0.0362(16) 0.083(2) -0.0245(16) -0.0047(14) -0.0014(12) C1 0.115(5) 0.072(4) 0.075(3) 0.000(3) -0.027(3) 0.008(3) C2 0.114(4) 0.047(3) 0.092(4) 0.001(2) -0.013(3) 0.011(3) C3 0.076(3) 0.044(2) 0.067(3) 0.000(2) 0.007(2) 0.003(2) C4 0.096(4) 0.036(2) 0.095(4) -0.016(2) 0.011(3) -0.011(2) C5 0.107(4) 0.047(3) 0.089(4) -0.027(2) 0.001(3) -0.020(3) C6 0.094(4) 0.048(2) 0.071(3) -0.018(2) -0.003(2) -0.015(2) C7 0.063(2) 0.0369(19) 0.056(2) -0.0105(17) 0.0045(18) -0.0049(17) C8 0.068(3) 0.040(2) 0.059(2) -0.0103(18) 0.005(2) -0.0060(18) C9 0.069(3) 0.040(2) 0.054(2) -0.0085(17) -0.0069(19) -0.0064(18) C10 0.055(2) 0.043(2) 0.054(2) -0.0116(17) -0.0063(18) -0.0070(17) C11 0.0315(19) 0.046(2) 0.081(3) -0.0196(19) -0.0060(17) -0.0084(15) C12 0.043(2) 0.040(2) 0.077(3) -0.0196(18) -0.0099(18) -0.0125(16) C13 0.0426(19) 0.0294(16) 0.0481(19) -0.0108(14) -0.0060(15) -0.0069(14) C14 0.058(2) 0.0261(17) 0.067(2) -0.0177(16) -0.0055(18) -0.0047(15) C15 0.052(2) 0.0331(19) 0.081(3) -0.0247(18) 0.0013(19) 0.0057(16) C16 0.0348(19) 0.0371(19) 0.074(2) -0.0151(17) -0.0026(17) 0.0001(15) C17 0.0321(17) 0.0287(16) 0.0493(19) -0.0124(14) -0.0030(14) -0.0025(13) C18 0.0347(17) 0.0282(16) 0.0447(18) -0.0094(13) -0.0049(14) -0.0035(13) C19 0.0247(16) 0.0366(18) 0.061(2) -0.0141(16) -0.0052(15) -0.0061(13) C20 0.0321(17) 0.0290(16) 0.0450(18) -0.0108(14) -0.0057(13) -0.0028(13) O1 0.099(3) 0.103(3) 0.104(3) -0.021(2) -0.025(2) 0.001(2) C21 0.236(10) 0.163(8) 0.064(4) -0.005(4) -0.028(5) -0.061(7) O2 0.240(7) 0.120(4) 0.119(4) -0.027(3) -0.079(4) -0.030(4) C22 0.142(6) 0.125(6) 0.094(4) -0.019(4) -0.039(4) -0.009(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 Br1 Zn1 2.3816(5) . Y Br2 Zn1 2.4154(6) . Y Zn1 S2 2.3398(10) . Y Zn1 S1 2.3650(11) . Y S1 C10 1.719(4) . Y S2 C20 1.712(3) . Y N1 C8 1.360(6) . ? N1 C1 1.389(6) . ? N1 H1N 0.851(19) . ? N2 C9 1.277(5) . Y N2 N3 1.384(4) . Y N3 C10 1.324(5) . Y N3 H3N 0.852(19) . ? N4 C10 1.312(5) . Y N4 H4A 0.864(19) . ? N4 H4B 0.833(19) . ? N5 C18 1.363(4) . ? N5 C11 1.377(4) . ? N5 H5N 0.851(18) . ? N6 C19 1.284(4) . Y N6 N7 1.380(3) . Y N7 C20 1.335(4) . Y N7 H7N 0.839(18) . ? N8 C20 1.308(4) . Y N8 H8A 0.853(19) . ? N8 H8B 0.843(18) . ? C1 C2 1.342(7) . ? C1 H1 0.9300 . ? C2 C3 1.418(7) . ? C2 H2 0.9300 . ? C3 C4 1.388(7) . ? C3 C8 1.427(5) . ? C4 C5 1.366(7) . ? C4 H4 0.9300 . ? C5 C6 1.395(6) . ? C5 H5 0.9300 . ? C6 C7 1.388(6) . ? C6 H6 0.9300 . ? C7 C8 1.393(6) . ? C7 C9 1.446(5) . ? C9 H9 0.9300 . ? C11 C12 1.340(5) . ? C11 H11 0.9300 . ? C12 C13 1.430(5) . ? C12 H12 0.9300 . ? C13 C14 1.393(5) . ? C13 C18 1.411(4) . ? C14 C15 1.380(5) . ? C14 H14 0.9300 . ? C15 C16 1.392(5) . ? C15 H15 0.9300 . ? C16 C17 1.389(4) . ? C16 H16 0.9300 . ? C17 C18 1.408(4) . ? C17 C19 1.441(4) . ? C19 H19 0.9300 . ? O1 C21 1.298(7) . ? O1 H1A 0.8200 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? O2 C22 1.334(7) . ? O2 H2A 0.8200 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 S2 Zn1 S1 110.59(4) . . Y S2 Zn1 Br1 107.04(3) . . Y S1 Zn1 Br1 112.03(3) . . Y S2 Zn1 Br2 113.14(3) . . Y S1 Zn1 Br2 100.26(3) . . Y Br1 Zn1 Br2 113.80(2) . . Y C10 S1 Zn1 106.96(13) . . Y C20 S2 Zn1 108.16(11) . . Y C8 N1 C1 108.4(4) . . ? C8 N1 H1N 132(3) . . ? C1 N1 H1N 119(3) . . ? C9 N2 N3 113.8(3) . . ? C10 N3 N2 121.3(3) . . ? C10 N3 H3N 118(3) . . ? N2 N3 H3N 121(3) . . ? C10 N4 H4A 119(3) . . ? C10 N4 H4B 122(3) . . ? H4A N4 H4B 119(5) . . ? C18 N5 C11 108.7(3) . . ? C18 N5 H5N 119(3) . . ? C11 N5 H5N 132(3) . . ? C19 N6 N7 113.7(3) . . ? C20 N7 N6 122.1(3) . . ? C20 N7 H7N 121(3) . . ? N6 N7 H7N 117(3) . . ? C20 N8 H8A 120(3) . . ? C20 N8 H8B 118(3) . . ? H8A N8 H8B 121(4) . . ? C2 C1 N1 109.5(5) . . ? C2 C1 H1 125.2 . . ? N1 C1 H1 125.2 . . ? C1 C2 C3 108.4(4) . . ? C1 C2 H2 125.8 . . ? C3 C2 H2 125.8 . . ? C4 C3 C2 135.0(4) . . ? C4 C3 C8 119.4(4) . . ? C2 C3 C8 105.7(4) . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.7(4) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 122.5(5) . . ? C7 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C6 C7 C8 116.4(4) . . ? C6 C7 C9 119.0(4) . . ? C8 C7 C9 124.5(4) . . ? N1 C8 C7 130.4(4) . . ? N1 C8 C3 108.0(4) . . ? C7 C8 C3 121.6(4) . . ? N2 C9 C7 124.1(4) . . ? N2 C9 H9 117.9 . . ? C7 C9 H9 117.9 . . ? N4 C10 N3 119.1(4) . . ? N4 C10 S1 119.8(3) . . ? N3 C10 S1 121.0(3) . . ? C12 C11 N5 110.2(3) . . ? C12 C11 H11 124.9 . . ? N5 C11 H11 124.9 . . ? C11 C12 C13 107.1(3) . . ? C11 C12 H12 126.4 . . ? C13 C12 H12 126.4 . . ? C14 C13 C18 118.9(3) . . ? C14 C13 C12 134.6(3) . . ? C18 C13 C12 106.5(3) . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 120.5(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 122.7(3) . . ? C17 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? C16 C17 C18 115.8(3) . . ? C16 C17 C19 120.3(3) . . ? C18 C17 C19 123.9(3) . . ? N5 C18 C17 129.9(3) . . ? N5 C18 C13 107.5(3) . . ? C17 C18 C13 122.6(3) . . ? N6 C19 C17 124.1(3) . . ? N6 C19 H19 118.0 . . ? C17 C19 H19 118.0 . . ? N8 C20 N7 119.0(3) . . ? N8 C20 S2 120.3(2) . . ? N7 C20 S2 120.8(2) . . ? C21 O1 H1A 109.5 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 O2 H2A 109.5 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N N2 0.851(19) 2.57(5) 2.955(5) 109(4) . N1 H1N O1 0.851(19) 2.07(3) 2.867(6) 155(5) . N3 H3N Br1 0.852(19) 2.61(2) 3.456(3) 171(4) . N4 H4A O1 0.864(19) 2.02(3) 2.804(6) 151(4) . N4 H4B O2 0.833(19) 2.09(2) 2.904(6) 166(5) . N5 H5N N6 0.851(18) 2.37(3) 2.930(4) 124(3) . N5 H5N Br2 0.851(18) 2.82(3) 3.361(3) 123(3) 1_455 N7 H7N Br2 0.839(18) 2.58(2) 3.399(3) 167(3) . N8 H8A Br2 0.853(19) 2.74(3) 3.434(3) 139(3) 1_455 N8 H8B Br1 0.843(18) 2.90(3) 3.625(3) 145(3) 1_455 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.734 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.066 loop_ _shelx_res_file ; TITL [Zn(LH2)2Br2] CELL 0.71073 8.2989 12.4402 14.7088 74.448 83.939 85.086 ZERR 2.00 0.0011 0.0016 0.0019 0.002 0.002 0.002 LATT 1 SFAC C H N S Zn Br O UNIT 44 56 16 4 2 4 4 OMIT -2 50.5 OMIT 0 1 0 L.S. 12 ACTA BOND $H DANG -2.4 H4B H2A SIZE 0.180 0.250 0.330 DFIX 0.86 N1 H1N N4 H4A N4 H4B N5 H5N N8 H8A N8 H8B N7 H7N N3 H3N TEMP 23.000 WGHT 0.047100 0.715700 FVAR 0.32178 BR1 6 1.084391 0.611095 0.849353 11.00000 0.05045 0.03438 = 0.08638 -0.01493 -0.02303 -0.01079 BR2 6 1.049878 0.285902 0.866466 11.00000 0.03135 0.02932 = 0.11307 -0.01318 -0.01588 0.00050 ZN1 5 0.927405 0.473644 0.821068 11.00000 0.03235 0.02634 = 0.06477 -0.01123 -0.00589 -0.00493 S1 4 0.912188 0.494886 0.657474 11.00000 0.07911 0.03616 = 0.06364 -0.01789 -0.01056 -0.00378 S2 4 0.668223 0.492276 0.897037 11.00000 0.03525 0.03269 = 0.08270 -0.02703 0.00328 -0.00858 N1 3 0.726214 1.028605 0.467628 11.00000 0.08838 0.04875 = 0.06747 -0.00668 -0.01640 0.00133 H1N 2 0.708896 0.962567 0.466412 11.00000 -1.20000 N2 3 0.843325 0.823449 0.604216 11.00000 0.06752 0.03448 = 0.05543 -0.00752 -0.00950 -0.00391 N3 3 0.886240 0.712397 0.645480 11.00000 0.06931 0.03330 = 0.05630 -0.00753 -0.01825 -0.00139 H3N 2 0.942654 0.693906 0.693039 11.00000 -1.20000 N4 3 0.769260 0.658117 0.533402 11.00000 0.09159 0.04814 = 0.07311 -0.01561 -0.03093 -0.00650 H4A 2 0.730999 0.726196 0.513069 11.00000 -1.20000 H4B 2 0.758336 0.612025 0.502885 11.00000 -1.20000 N5 3 0.289905 0.049626 0.894825 11.00000 0.03434 0.02902 = 0.06925 -0.01756 -0.00742 -0.00356 H5N 2 0.301066 0.115872 0.897913 11.00000 -1.20000 N6 3 0.555190 0.194988 0.883266 11.00000 0.02959 0.02749 = 0.05331 -0.01167 -0.00483 -0.00725 N7 3 0.638140 0.286195 0.884047 11.00000 0.02462 0.02967 = 0.06932 -0.01783 -0.00554 -0.00434 H7N 2 0.738942 0.275962 0.886947 11.00000 -1.20000 N8 3 0.402590 0.390440 0.899654 11.00000 0.02875 0.03621 = 0.08297 -0.02448 -0.00470 -0.00140 H8A 2 0.349054 0.333694 0.903260 11.00000 -1.20000 H8B 2 0.355474 0.451491 0.905062 11.00000 -1.20000 C1 1 0.668443 1.119011 0.398346 11.00000 0.11549 0.07234 = 0.07488 -0.00020 -0.02739 0.00751 AFIX 43 H1 2 0.617527 1.114106 0.346349 11.00000 -1.20000 AFIX 0 C2 1 0.697412 1.214511 0.417996 11.00000 0.11363 0.04691 = 0.09208 0.00062 -0.01292 0.01055 AFIX 43 H2 2 0.670610 1.286278 0.381931 11.00000 -1.20000 AFIX 0 C3 1 0.775820 1.187480 0.503071 11.00000 0.07636 0.04414 = 0.06679 0.00014 0.00655 0.00280 C4 1 0.835203 1.248678 0.557104 11.00000 0.09557 0.03610 = 0.09469 -0.01614 0.01106 -0.01108 AFIX 43 H4 2 0.823271 1.326332 0.539785 11.00000 -1.20000 AFIX 0 C5 1 0.911319 1.193894 0.635931 11.00000 0.10656 0.04715 = 0.08944 -0.02740 0.00103 -0.02000 AFIX 43 H5 2 0.951722 1.234653 0.672144 11.00000 -1.20000 AFIX 0 C6 1 0.929088 1.077382 0.662695 11.00000 0.09367 0.04774 = 0.07141 -0.01755 -0.00302 -0.01457 AFIX 43 H6 2 0.982349 1.042402 0.716386 11.00000 -1.20000 AFIX 0 C7 1 0.870274 1.011706 0.612212 11.00000 0.06254 0.03694 = 0.05588 -0.01048 0.00447 -0.00492 C8 1 0.792650 1.068294 0.531944 11.00000 0.06755 0.03995 = 0.05867 -0.01029 0.00481 -0.00598 C9 1 0.895631 0.891490 0.644006 11.00000 0.06878 0.04017 = 0.05384 -0.00849 -0.00694 -0.00644 AFIX 43 H9 2 0.953685 0.861892 0.696749 11.00000 -1.20000 AFIX 0 C10 1 0.849919 0.631880 0.609177 11.00000 0.05540 0.04336 = 0.05398 -0.01160 -0.00630 -0.00703 C11 1 0.154346 -0.008847 0.899721 11.00000 0.03149 0.04623 = 0.08141 -0.01960 -0.00598 -0.00837 AFIX 43 H11 2 0.047822 0.019751 0.906618 11.00000 -1.20000 AFIX 0 C12 1 0.197947 -0.112900 0.893120 11.00000 0.04333 0.03995 = 0.07670 -0.01956 -0.00987 -0.01248 AFIX 43 H12 2 0.128435 -0.168208 0.894459 11.00000 -1.20000 AFIX 0 C13 1 0.371489 -0.122896 0.883627 11.00000 0.04256 0.02939 = 0.04809 -0.01077 -0.00602 -0.00685 C14 1 0.486898 -0.208893 0.876065 11.00000 0.05791 0.02610 = 0.06717 -0.01773 -0.00547 -0.00467 AFIX 43 H14 2 0.454535 -0.277746 0.873640 11.00000 -1.20000 AFIX 0 C15 1 0.649667 -0.191123 0.872198 11.00000 0.05177 0.03307 = 0.08102 -0.02470 0.00131 0.00565 AFIX 43 H15 2 0.727032 -0.248743 0.868269 11.00000 -1.20000 AFIX 0 C16 1 0.698928 -0.087662 0.874132 11.00000 0.03484 0.03708 = 0.07378 -0.01512 -0.00262 0.00012 AFIX 43 H16 2 0.809399 -0.078139 0.871578 11.00000 -1.20000 AFIX 0 C17 1 0.589910 0.001947 0.879717 11.00000 0.03214 0.02868 = 0.04931 -0.01239 -0.00304 -0.00245 C18 1 0.424535 -0.018950 0.885946 11.00000 0.03470 0.02818 = 0.04471 -0.00935 -0.00494 -0.00353 C19 1 0.647820 0.107525 0.880710 11.00000 0.02473 0.03656 = 0.06147 -0.01409 -0.00520 -0.00613 AFIX 43 H19 2 0.759224 0.112640 0.879420 11.00000 -1.20000 AFIX 0 C20 1 0.561381 0.382236 0.892671 11.00000 0.03208 0.02902 = 0.04501 -0.01080 -0.00566 -0.00284 O1 7 0.601751 0.843564 0.421438 11.00000 0.09853 0.10273 = 0.10356 -0.02058 -0.02500 0.00063 AFIX 147 H1A 2 0.511243 0.829242 0.448027 11.00000 -1.50000 AFIX 0 C21 1 0.598059 0.858381 0.330855 11.00000 0.23570 0.16287 = 0.06364 -0.00467 -0.02826 -0.06088 AFIX 137 H21A 2 0.547197 0.930623 0.304024 11.00000 -1.50000 H21B 2 0.537405 0.801576 0.319586 11.00000 -1.50000 H21C 2 0.706846 0.853899 0.301986 11.00000 -1.50000 AFIX 0 O2 7 0.680620 0.519285 0.418358 11.00000 0.23969 0.11952 = 0.11930 -0.02743 -0.07944 -0.03002 AFIX 147 H2A 2 0.638603 0.473592 0.463795 11.00000 -1.50000 AFIX 0 C22 1 0.581175 0.547256 0.349021 11.00000 0.14174 0.12465 = 0.09377 -0.01868 -0.03922 -0.00876 AFIX 137 H22A 2 0.471513 0.555575 0.375536 11.00000 -1.50000 H22B 2 0.589347 0.489748 0.316091 11.00000 -1.50000 H22C 2 0.611119 0.616570 0.305553 11.00000 -1.50000 HKLF 4 REM sad in P-1 REM R1 = 0.0322 for 4116 Fo > 4sig(Fo) and 0.0430 for all 5109 data REM 362 parameters refined using 9 restraints END WGHT 0.0466 0.7674 REM Highest difference peak 0.734, deepest hole -0.688, 1-sigma level 0.066 Q1 1 0.5504 0.5561 0.4454 11.00000 0.05 0.73 Q2 1 0.7216 0.8505 0.3606 11.00000 0.05 0.51 Q3 1 1.0847 0.5618 0.8162 11.00000 0.05 0.37 Q4 1 1.1100 0.3250 0.8189 11.00000 0.05 0.33 ; _database_code_depnum_ccdc_archive 'CCDC 939908' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[Cd(LH2)2Cl2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 Cd Cl2 N8 S2, C H4 O' _chemical_formula_sum 'C21 H24 Cd Cl2 N8 O S2' _chemical_formula_weight 651.90 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' Cd Cd -0.8075 1.2024 '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' 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 14.293(7) _cell_length_b 15.549(8) _cell_length_c 12.519(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.673(9) _cell_angle_gamma 90.00 _cell_volume 2781(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6977 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.29 _exptl_crystal_description Rod _exptl_crystal_colour pink _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.157 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6181 _exptl_absorpt_correction_T_max 0.8548 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16726 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6313 _reflns_number_gt 4827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0383P)^2^+0.6880P] 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 6313 _refine_ls_number_parameters 357 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _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 Cd1 Cd 0.823830(13) 0.361210(14) 0.573443(13) 0.04676(8) Uani 1 1 d . . . Cl1 Cl 0.95122(4) 0.37970(4) 0.71426(5) 0.04705(16) Uani 1 1 d . . . Cl2 Cl 0.82620(5) 0.20507(5) 0.53951(5) 0.05213(17) Uani 1 1 d . . . S1 S 0.67171(6) 0.42632(7) 0.63149(5) 0.0750(3) Uani 1 1 d . . . S2 S 0.86164(6) 0.44649(5) 0.41022(5) 0.0587(2) Uani 1 1 d . . . N1 N 0.62328(16) 0.35193(18) 1.14478(18) 0.0604(7) Uani 1 1 d . . . H1N H 0.6581 0.3579 1.0904 0.073 Uiso 1 1 calc R . . N2 N 0.57352(15) 0.38817(17) 0.91726(15) 0.0509(6) Uani 1 1 d . . . N3 N 0.58194(16) 0.40439(19) 0.80832(16) 0.0583(7) Uani 1 1 d D . . H3N H 0.5322(16) 0.409(2) 0.766(2) 0.070 Uiso 1 1 d D . . N4 N 0.74112(17) 0.3879(2) 0.82737(18) 0.0669(8) Uani 1 1 d D . . H4A H 0.736(2) 0.368(2) 0.8903(17) 0.080 Uiso 1 1 d D . . H4B H 0.7971(14) 0.389(2) 0.807(3) 0.080 Uiso 1 1 d D . . N5 N 1.09288(15) 0.23906(15) 0.05156(17) 0.0491(5) Uani 1 1 d . . . H5N H 1.0623 0.2406 0.1097 0.059 Uiso 1 1 calc R . . N6 N 1.02393(14) 0.38053(14) 0.17676(15) 0.0410(5) Uani 1 1 d . . . N7 N 0.97492(15) 0.42490(15) 0.25394(16) 0.0457(5) Uani 1 1 d D . . H7N H 0.9758(19) 0.4801(11) 0.255(2) 0.055 Uiso 1 1 d D . . N8 N 0.92836(19) 0.29992(17) 0.33117(18) 0.0559(6) Uani 1 1 d D . . H8A H 0.9635(19) 0.2698(18) 0.291(2) 0.067 Uiso 1 1 d D . . H8B H 0.899(2) 0.2707(18) 0.378(2) 0.067 Uiso 1 1 d D . . C1 C 0.6549(2) 0.3354(3) 1.2481(2) 0.0754(10) Uani 1 1 d . . . H1 H 0.7173 0.3281 1.2696 0.090 Uiso 1 1 calc R . . C2 C 0.5810(2) 0.3314(3) 1.3132(2) 0.0715(9) Uani 1 1 d . . . H2 H 0.5839 0.3223 1.3866 0.086 Uiso 1 1 calc R . . C3 C 0.4975(2) 0.3437(2) 1.2487(2) 0.0551(7) Uani 1 1 d . . . C4 C 0.4015(2) 0.3446(2) 1.2689(2) 0.0716(10) Uani 1 1 d . . . H4 H 0.3809 0.3358 1.3379 0.086 Uiso 1 1 calc R . . C5 C 0.3381(2) 0.3585(3) 1.1859(2) 0.0791(11) Uani 1 1 d . . . H5 H 0.2744 0.3587 1.1993 0.095 Uiso 1 1 calc R . . C6 C 0.3678(2) 0.3723(2) 1.0819(2) 0.0674(10) Uani 1 1 d . . . H6 H 0.3232 0.3818 1.0275 0.081 Uiso 1 1 calc R . . C7 C 0.46273(18) 0.3722(2) 1.05723(19) 0.0511(7) Uani 1 1 d . . . C8 C 0.52758(18) 0.35720(18) 1.14279(19) 0.0469(6) Uani 1 1 d . . . C9 C 0.48803(18) 0.3879(2) 0.94740(19) 0.0545(7) Uani 1 1 d . . . H9 H 0.4405 0.3982 0.8966 0.065 Uiso 1 1 calc R . . C10 C 0.66681(19) 0.4039(2) 0.76608(19) 0.0528(7) Uani 1 1 d . . . C11 C 1.1198(2) 0.1660(2) 0.0005(3) 0.0640(8) Uani 1 1 d . . . H11 H 1.1073 0.1102 0.0229 0.077 Uiso 1 1 calc R . . C12 C 1.1678(2) 0.1873(2) -0.0883(2) 0.0628(8) Uani 1 1 d . . . H12 H 1.1941 0.1490 -0.1360 0.075 Uiso 1 1 calc R . . C13 C 1.17004(17) 0.2777(2) -0.09475(19) 0.0473(7) Uani 1 1 d . . . C14 C 1.20721(18) 0.3382(2) -0.1657(2) 0.0535(7) Uani 1 1 d . . . H14 H 1.2386 0.3197 -0.2256 0.064 Uiso 1 1 calc R . . C15 C 1.19686(18) 0.4241(2) -0.1462(2) 0.0543(7) Uani 1 1 d . . . H15 H 1.2220 0.4637 -0.1931 0.065 Uiso 1 1 calc R . . C16 C 1.14905(18) 0.4543(2) -0.05658(19) 0.0480(6) Uani 1 1 d . . . H16 H 1.1427 0.5132 -0.0460 0.058 Uiso 1 1 calc R . . C17 C 1.11097(16) 0.39689(17) 0.01664(17) 0.0384(5) Uani 1 1 d . . . C18 C 1.12194(16) 0.30940(18) -0.00394(17) 0.0404(6) Uani 1 1 d . . . C19 C 1.06083(16) 0.43041(17) 0.10664(18) 0.0414(6) Uani 1 1 d . . . H19 H 1.0550 0.4896 0.1143 0.050 Uiso 1 1 calc R . . C20 C 0.92688(18) 0.38306(17) 0.32836(18) 0.0415(6) Uani 1 1 d . . . O1 O 0.4129(2) 0.4464(4) 0.6918(3) 0.0827(17) Uani 0.830(11) 1 d P A 1 H1A H 0.4234 0.4971 0.6792 0.124 Uiso 0.830(11) 1 calc PR A 1 C21 C 0.3925(11) 0.4021(10) 0.5943(12) 0.135(6) Uani 0.830(11) 1 d P A 1 H21A H 0.3290 0.4136 0.5715 0.203 Uiso 0.830(11) 1 calc PR A 1 H21B H 0.4006 0.3414 0.6051 0.203 Uiso 0.830(11) 1 calc PR A 1 H21C H 0.4341 0.4215 0.5406 0.203 Uiso 0.830(11) 1 calc PR A 1 O1' O 0.4135(12) 0.368(2) 0.6785(14) 0.086(9) Uani 0.170(11) 1 d P A 2 H1' H 0.4693 0.3605 0.6681 0.129 Uiso 0.170(11) 1 calc PR A 2 C21' C 0.379(5) 0.409(4) 0.606(4) 0.087(17) Uani 0.170(11) 1 d P A 2 H21D H 0.3428 0.4556 0.6341 0.131 Uiso 0.170(11) 1 calc PR A 2 H21E H 0.3394 0.3729 0.5625 0.131 Uiso 0.170(11) 1 calc PR A 2 H21F H 0.4279 0.4325 0.5632 0.131 Uiso 0.170(11) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.05172(12) 0.05608(15) 0.03325(10) -0.00109(8) 0.01433(7) -0.00148(9) Cl1 0.0505(4) 0.0459(4) 0.0452(3) -0.0039(3) 0.0081(3) -0.0079(3) Cl2 0.0555(4) 0.0532(4) 0.0479(3) -0.0026(3) 0.0064(3) -0.0124(3) S1 0.0653(5) 0.1261(8) 0.0346(3) 0.0229(4) 0.0197(3) 0.0372(5) S2 0.0885(5) 0.0459(4) 0.0436(3) 0.0018(3) 0.0334(3) 0.0069(4) N1 0.0429(12) 0.095(2) 0.0440(12) 0.0012(12) 0.0067(9) 0.0055(12) N2 0.0483(12) 0.0754(17) 0.0295(9) 0.0053(10) 0.0112(8) 0.0068(11) N3 0.0459(13) 0.098(2) 0.0314(10) 0.0110(12) 0.0109(9) 0.0118(13) N4 0.0453(13) 0.121(2) 0.0352(11) 0.0165(13) 0.0145(10) 0.0122(14) N5 0.0556(13) 0.0449(14) 0.0481(11) 0.0071(10) 0.0225(10) 0.0039(10) N6 0.0463(11) 0.0440(13) 0.0335(9) -0.0003(8) 0.0132(8) 0.0004(9) N7 0.0617(13) 0.0369(13) 0.0397(10) -0.0030(9) 0.0214(9) -0.0033(10) N8 0.0790(17) 0.0428(15) 0.0477(12) -0.0030(10) 0.0335(11) -0.0054(12) C1 0.0533(18) 0.116(3) 0.0566(18) -0.0006(18) -0.0074(14) 0.0108(18) C2 0.074(2) 0.101(3) 0.0392(14) 0.0036(16) 0.0000(14) 0.0084(19) C3 0.0590(17) 0.069(2) 0.0375(13) 0.0003(12) 0.0097(11) 0.0013(14) C4 0.0624(19) 0.112(3) 0.0412(14) 0.0084(16) 0.0201(13) -0.0006(18) C5 0.0474(17) 0.139(4) 0.0517(17) 0.0082(19) 0.0205(13) -0.0012(18) C6 0.0398(15) 0.119(3) 0.0439(14) 0.0102(16) 0.0088(11) 0.0046(16) C7 0.0419(14) 0.077(2) 0.0354(12) 0.0021(12) 0.0110(10) 0.0011(13) C8 0.0442(14) 0.0590(19) 0.0379(12) -0.0025(12) 0.0103(10) 0.0025(12) C9 0.0415(14) 0.087(2) 0.0355(12) 0.0055(13) 0.0076(10) 0.0049(13) C10 0.0492(15) 0.075(2) 0.0349(12) 0.0096(12) 0.0138(10) 0.0154(14) C11 0.072(2) 0.0477(19) 0.0737(19) 0.0053(15) 0.0275(16) 0.0110(15) C12 0.0648(19) 0.061(2) 0.0639(18) -0.0097(15) 0.0258(14) 0.0111(14) C13 0.0407(13) 0.063(2) 0.0383(12) -0.0009(12) 0.0109(10) 0.0044(11) C14 0.0489(15) 0.078(2) 0.0346(12) 0.0051(13) 0.0147(10) 0.0051(14) C15 0.0517(15) 0.072(2) 0.0400(13) 0.0171(13) 0.0151(11) 0.0000(14) C16 0.0479(14) 0.0543(18) 0.0422(12) 0.0115(12) 0.0087(10) -0.0028(12) C17 0.0350(12) 0.0471(16) 0.0335(11) 0.0052(10) 0.0075(9) 0.0006(10) C18 0.0361(12) 0.0513(17) 0.0342(11) 0.0056(11) 0.0081(9) 0.0016(11) C19 0.0455(13) 0.0412(15) 0.0380(11) 0.0017(10) 0.0093(10) -0.0009(11) C20 0.0502(14) 0.0426(16) 0.0322(11) -0.0020(10) 0.0113(10) -0.0031(11) O1 0.078(2) 0.104(4) 0.066(2) 0.0134(19) -0.0059(15) 0.016(2) C21 0.122(10) 0.203(13) 0.080(7) -0.021(6) -0.018(6) -0.018(8) O1' 0.076(10) 0.11(2) 0.069(11) 0.013(10) 0.001(8) -0.007(10) C21' 0.09(2) 0.12(3) 0.06(2) 0.05(2) -0.002(17) 0.04(2) _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 Cd1 Cl2 2.4651(14) . Y Cd1 S2 2.5080(11) . Y Cd1 Cl1 2.5137(11) . Y Cd1 S1 2.5245(12) . Y S1 C10 1.724(3) . Y S2 C20 1.717(3) . Y N1 C8 1.370(3) . ? N1 C1 1.382(4) . ? N1 H1N 0.8600 . ? N2 C9 1.289(3) . Y N2 N3 1.396(3) . Y N3 C10 1.337(3) . Y N3 H3N 0.878(17) . ? N4 C10 1.316(4) . Y N4 H4A 0.848(18) . ? N4 H4B 0.849(18) . ? N5 C11 1.364(4) . ? N5 C18 1.367(3) . ? N5 H5N 0.8600 . ? N6 C19 1.295(3) . Y N6 N7 1.393(3) . Y N7 C20 1.342(3) . Y N7 H7N 0.858(17) . ? N8 C20 1.293(4) . Y N8 H8A 0.860(17) . ? N8 H8B 0.856(17) . ? C1 C2 1.355(4) . ? C1 H1 0.9300 . ? C2 C3 1.434(4) . ? C2 H2 0.9300 . ? C3 C4 1.402(4) . ? C3 C8 1.422(3) . ? C4 C5 1.376(5) . ? C4 H4 0.9300 . ? C5 C6 1.399(4) . ? C5 H5 0.9300 . ? C6 C7 1.401(4) . ? C6 H6 0.9300 . ? C7 C8 1.415(4) . ? C7 C9 1.452(3) . ? C9 H9 0.9300 . ? C11 C12 1.364(4) . ? C11 H11 0.9300 . ? C12 C13 1.409(5) . ? C12 H12 0.9300 . ? C13 C14 1.409(4) . ? C13 C18 1.433(3) . ? C14 C15 1.368(4) . ? C14 H14 0.9300 . ? C15 C16 1.411(4) . ? C15 H15 0.9300 . ? C16 C17 1.401(3) . ? C16 H16 0.9300 . ? C17 C18 1.394(4) . ? C17 C19 1.450(3) . ? C19 H19 0.9300 . ? O1 C21 1.424(16) . ? O1 H1A 0.8200 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? O1' C21' 1.21(5) . ? O1' H1' 0.8200 . ? C21' H21D 0.9600 . ? C21' H21E 0.9600 . ? C21' H21F 0.9600 . ? 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 Cl2 Cd1 S2 112.08(3) . . Y Cl2 Cd1 Cl1 102.72(2) . . Y S2 Cd1 Cl1 110.00(4) . . Y Cl2 Cd1 S1 117.44(3) . . Y S2 Cd1 S1 103.32(3) . . Y Cl1 Cd1 S1 111.39(4) . . Y C10 S1 Cd1 105.07(9) . . Y C20 S2 Cd1 108.44(10) . . Y C8 N1 C1 109.1(2) . . ? C8 N1 H1N 125.4 . . ? C1 N1 H1N 125.4 . . ? C9 N2 N3 113.3(2) . . ? C10 N3 N2 119.4(2) . . ? C10 N3 H3N 119(2) . . ? N2 N3 H3N 121(2) . . ? C10 N4 H4A 121(2) . . ? C10 N4 H4B 125(2) . . ? H4A N4 H4B 113(3) . . ? C11 N5 C18 109.5(2) . . ? C11 N5 H5N 125.2 . . ? C18 N5 H5N 125.2 . . ? C19 N6 N7 113.4(2) . . ? C20 N7 N6 121.3(2) . . ? C20 N7 H7N 118.7(19) . . ? N6 N7 H7N 120.0(19) . . ? C20 N8 H8A 123(2) . . ? C20 N8 H8B 123(2) . . ? H8A N8 H8B 114(3) . . ? C2 C1 N1 109.4(3) . . ? C2 C1 H1 125.3 . . ? N1 C1 H1 125.3 . . ? C1 C2 C3 107.9(3) . . ? C1 C2 H2 126.1 . . ? C3 C2 H2 126.1 . . ? C4 C3 C8 119.4(3) . . ? C4 C3 C2 134.6(3) . . ? C8 C3 C2 105.9(2) . . ? C5 C4 C3 119.5(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.1(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 121.9(3) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C8 116.8(2) . . ? C6 C7 C9 118.6(2) . . ? C8 C7 C9 124.6(2) . . ? N1 C8 C7 130.9(2) . . ? N1 C8 C3 107.7(2) . . ? C7 C8 C3 121.4(2) . . ? N2 C9 C7 122.8(2) . . ? N2 C9 H9 118.6 . . ? C7 C9 H9 118.6 . . ? N4 C10 N3 119.8(2) . . ? N4 C10 S1 123.57(19) . . ? N3 C10 S1 116.6(2) . . ? N5 C11 C12 109.6(3) . . ? N5 C11 H11 125.2 . . ? C12 C11 H11 125.2 . . ? C11 C12 C13 107.6(3) . . ? C11 C12 H12 126.2 . . ? C13 C12 H12 126.2 . . ? C14 C13 C12 135.4(2) . . ? C14 C13 C18 118.0(3) . . ? C12 C13 C18 106.6(2) . . ? C15 C14 C13 119.6(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 121.7(2) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C17 C16 C15 120.9(3) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C18 C17 C16 117.0(2) . . ? C18 C17 C19 123.7(2) . . ? C16 C17 C19 119.3(2) . . ? N5 C18 C17 130.5(2) . . ? N5 C18 C13 106.7(2) . . ? C17 C18 C13 122.8(2) . . ? N6 C19 C17 122.1(2) . . ? N6 C19 H19 118.9 . . ? C17 C19 H19 118.9 . . ? N8 C20 N7 119.7(2) . . ? N8 C20 S2 124.51(18) . . ? N7 C20 S2 115.7(2) . . ? C21' O1' H1' 109.5 . . ? O1' C21' H21D 109.5 . . ? O1' C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? O1' C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N N2 0.86 2.50 2.970(3) 115.5 . N1 H1N Cl2 0.86 2.69 3.340(3) 133.6 4_566 N3 H3N O1 0.878(17) 2.003(19) 2.861(4) 165(3) . N3 H3N O1' 0.878(17) 2.09(3) 2.919(19) 157(3) . N4 H4A Cl2 0.848(18) 2.51(3) 3.230(3) 143(3) 4_566 N4 H4B Cl1 0.849(18) 2.521(19) 3.360(3) 170(3) . N5 H5N N6 0.86 2.40 2.891(3) 116.6 . N5 H5N Cl1 0.86 2.80 3.449(2) 133.2 4_565 N7 H7N Cl1 0.858(17) 2.44(2) 3.237(3) 154(2) 3_766 N8 H8A Cl1 0.860(17) 2.52(3) 3.174(3) 134(3) 4_565 N8 H8B Cl2 0.856(17) 2.521(18) 3.366(2) 169(3) . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.476 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.074 loop_ _shelx_res_file ; TITL [Cd(LH2)2Cl2] CELL 0.71073 14.2935 15.5493 12.5187 90.000 91.673 90.000 ZERR 4.00 0.0074 0.0076 0.0057 0.000 0.009 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H Cd Cl N O S UNIT 84 96 4 8 32 4 8 OMIT 1 1 0 OMIT 1 0 0 OMIT 0 16 0 OMIT 1 14 2 OMIT -1 15 2 OMIT 2 8 1 OMIT 5 15 0 OMIT -3 17 2 OMIT -2 55 L.S. 10 ACTA BOND $H SIZE 0.14 0.18 0.46 DFIX 0.86 N3 H3N N4 H4A N4 H4B N8 H8A N8 H8B N7 H7N TEMP 23.000 WGHT 0.038300 0.688000 FVAR 0.06591 0.82950 CD1 3 0.823830 0.361210 0.573443 11.00000 0.05172 0.05608 = 0.03325 -0.00109 0.01433 -0.00148 CL1 4 0.951222 0.379699 0.714264 11.00000 0.05048 0.04585 = 0.04521 -0.00394 0.00814 -0.00786 CL2 4 0.826203 0.205072 0.539514 11.00000 0.05549 0.05323 = 0.04794 -0.00259 0.00639 -0.01241 S1 7 0.671706 0.426322 0.631488 11.00000 0.06534 0.12609 = 0.03464 0.02285 0.01965 0.03715 S2 7 0.861644 0.446488 0.410221 11.00000 0.08854 0.04587 = 0.04361 0.00181 0.03344 0.00685 N1 5 0.623278 0.351929 1.144784 11.00000 0.04287 0.09479 = 0.04396 0.00120 0.00671 0.00551 AFIX 43 H1N 2 0.658098 0.357946 1.090410 11.00000 -1.20000 AFIX 0 N2 5 0.573516 0.388168 0.917255 11.00000 0.04835 0.07542 = 0.02952 0.00526 0.01122 0.00678 N3 5 0.581936 0.404394 0.808322 11.00000 0.04594 0.09806 = 0.03143 0.01102 0.01094 0.01180 H3N 2 0.532194 0.409131 0.765895 11.00000 -1.20000 N4 5 0.741123 0.387906 0.827373 11.00000 0.04529 0.12095 = 0.03519 0.01648 0.01454 0.01221 H4A 2 0.736124 0.368442 0.890254 11.00000 -1.20000 H4B 2 0.797150 0.388731 0.806614 11.00000 -1.20000 N5 5 1.092878 0.239057 0.051563 11.00000 0.05564 0.04486 = 0.04806 0.00711 0.02250 0.00385 AFIX 43 H5N 2 1.062330 0.240623 0.109706 11.00000 -1.20000 AFIX 0 N6 5 1.023930 0.380525 0.176757 11.00000 0.04631 0.04401 = 0.03350 -0.00032 0.01322 0.00044 N7 5 0.974916 0.424896 0.253939 11.00000 0.06168 0.03695 = 0.03969 -0.00302 0.02139 -0.00328 H7N 2 0.975764 0.480086 0.255115 11.00000 -1.20000 N8 5 0.928356 0.299919 0.331169 11.00000 0.07905 0.04275 = 0.04774 -0.00299 0.03347 -0.00543 H8A 2 0.963527 0.269817 0.291050 11.00000 -1.20000 H8B 2 0.899356 0.270691 0.377820 11.00000 -1.20000 C1 1 0.654939 0.335400 1.248091 11.00000 0.05325 0.11579 = 0.05662 -0.00063 -0.00735 0.01075 AFIX 43 H1 2 0.717274 0.328145 1.269572 11.00000 -1.20000 AFIX 0 C2 1 0.581014 0.331412 1.313194 11.00000 0.07416 0.10111 = 0.03920 0.00359 0.00002 0.00836 AFIX 43 H2 2 0.583912 0.322344 1.386647 11.00000 -1.20000 AFIX 0 C3 1 0.497471 0.343658 1.248720 11.00000 0.05897 0.06923 = 0.03746 0.00025 0.00967 0.00130 C4 1 0.401484 0.344575 1.268931 11.00000 0.06241 0.11219 = 0.04124 0.00843 0.02008 -0.00057 AFIX 43 H4 2 0.380871 0.335839 1.337870 11.00000 -1.20000 AFIX 0 C5 1 0.338056 0.358502 1.185949 11.00000 0.04735 0.13938 = 0.05174 0.00821 0.02047 -0.00118 AFIX 43 H5 2 0.274386 0.358734 1.199272 11.00000 -1.20000 AFIX 0 C6 1 0.367775 0.372317 1.081889 11.00000 0.03978 0.11903 = 0.04386 0.01017 0.00877 0.00462 AFIX 43 H6 2 0.323235 0.381820 1.027532 11.00000 -1.20000 AFIX 0 C7 1 0.462732 0.372243 1.057232 11.00000 0.04187 0.07674 = 0.03542 0.00206 0.01104 0.00106 C8 1 0.527582 0.357203 1.142794 11.00000 0.04424 0.05905 = 0.03794 -0.00246 0.01026 0.00246 C9 1 0.488034 0.387894 0.947399 11.00000 0.04155 0.08698 = 0.03548 0.00553 0.00762 0.00489 AFIX 43 H9 2 0.440539 0.398157 0.896642 11.00000 -1.20000 AFIX 0 C10 1 0.666807 0.403888 0.766083 11.00000 0.04922 0.07511 = 0.03486 0.00964 0.01382 0.01539 C11 1 1.119788 0.165976 0.000534 11.00000 0.07195 0.04771 = 0.07369 0.00534 0.02749 0.01104 AFIX 43 H11 2 1.107344 0.110207 0.022896 11.00000 -1.20000 AFIX 0 C12 1 1.167753 0.187260 -0.088331 11.00000 0.06483 0.06097 = 0.06394 -0.00966 0.02580 0.01108 AFIX 43 H12 2 1.194139 0.149024 -0.135995 11.00000 -1.20000 AFIX 0 C13 1 1.170043 0.277694 -0.094754 11.00000 0.04073 0.06346 = 0.03834 -0.00093 0.01095 0.00437 C14 1 1.207215 0.338168 -0.165746 11.00000 0.04891 0.07771 = 0.03461 0.00511 0.01474 0.00506 AFIX 43 H14 2 1.238631 0.319747 -0.225606 11.00000 -1.20000 AFIX 0 C15 1 1.196859 0.424118 -0.146174 11.00000 0.05174 0.07188 = 0.03998 0.01707 0.01512 -0.00003 AFIX 43 H15 2 1.221979 0.463664 -0.193130 11.00000 -1.20000 AFIX 0 C16 1 1.149046 0.454342 -0.056582 11.00000 0.04794 0.05434 = 0.04225 0.01148 0.00868 -0.00279 AFIX 43 H16 2 1.142708 0.513227 -0.045973 11.00000 -1.20000 AFIX 0 C17 1 1.110972 0.396888 0.016645 11.00000 0.03503 0.04706 = 0.03346 0.00519 0.00747 0.00057 C18 1 1.121938 0.309402 -0.003937 11.00000 0.03612 0.05129 = 0.03420 0.00556 0.00807 0.00157 C19 1 1.060825 0.430412 0.106637 11.00000 0.04554 0.04116 = 0.03799 0.00174 0.00928 -0.00088 AFIX 43 H19 2 1.054961 0.489645 0.114259 11.00000 -1.20000 AFIX 0 C20 1 0.926882 0.383064 0.328360 11.00000 0.05022 0.04261 = 0.03220 -0.00199 0.01130 -0.00312 PART 1 O1 6 0.412853 0.446367 0.691848 21.00000 0.07782 0.10350 = 0.06634 0.01344 -0.00587 0.01565 AFIX 147 H1A 2 0.423380 0.497135 0.679169 21.00000 -1.50000 AFIX 0 C21 1 0.392464 0.402120 0.594340 21.00000 0.12213 0.20311 = 0.08001 -0.02076 -0.01755 -0.01789 AFIX 137 H21A 2 0.328969 0.413558 0.571547 21.00000 -1.50000 H21B 2 0.400581 0.341423 0.605147 21.00000 -1.50000 H21C 2 0.434097 0.421549 0.540585 21.00000 -1.50000 AFIX 0 PART 2 O1' 6 0.413546 0.368089 0.678535 -21.00000 0.07630 0.11330 = 0.06862 0.01267 0.00127 -0.00695 AFIX 147 H1' 2 0.469319 0.360518 0.668130 -21.00000 -1.50000 AFIX 0 C21' 1 0.379160 0.409360 0.605893 -21.00000 0.08733 0.11750 = 0.05711 0.04764 -0.00228 0.04249 AFIX 137 H21D 2 0.342818 0.455555 0.634146 -21.00000 -1.50000 H21E 2 0.339432 0.372857 0.562507 -21.00000 -1.50000 H21F 2 0.427857 0.432523 0.563197 -21.00000 -1.50000 PART 0 HKLF 4 REM 1 in P2(1)/c REM R1 = 0.0292 for 4827 Fo > 4sig(Fo) and 0.0455 for all 6313 data REM 357 parameters refined using 6 restraints END WGHT 0.0305 0.7919 REM Highest difference peak 0.476, deepest hole -0.482, 1-sigma level 0.074 Q1 1 0.7815 0.2360 0.5187 11.00000 0.05 0.48 Q2 1 0.9198 0.4440 0.4422 11.00000 0.05 0.37 Q3 1 0.6252 0.4490 0.6226 11.00000 0.05 0.28 Q4 1 1.1566 0.3073 -0.0395 11.00000 0.05 0.28 ; _database_code_depnum_ccdc_archive 'CCDC 939909' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[Cd(LH2)2(OAc)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 Cd N8 O4 S2, 2(C H4 O)' _chemical_formula_sum 'C26 H34 Cd N8 O6 S2' _chemical_formula_weight 731.13 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' Cd Cd -0.8075 1.2024 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.223(7) _cell_length_b 14.649(9) _cell_length_c 19.869(11) _cell_angle_alpha 83.91(3) _cell_angle_beta 80.87(3) _cell_angle_gamma 77.10(4) _cell_volume 3415(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2468 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 20.86 _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.810 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8881 _exptl_absorpt_correction_T_max 0.9761 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19610 _diffrn_reflns_av_R_equivalents 0.0908 _diffrn_reflns_av_sigmaI/netI 0.1852 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 25.25 _reflns_number_total 12116 _reflns_number_gt 5254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0976P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12116 _refine_ls_number_parameters 787 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1902 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2349 _refine_ls_wR_factor_gt 0.1848 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 Cd1 Cd -0.06038(6) 0.33169(6) 0.25918(4) 0.0660(3) Uani 1 1 d . . . S1 S -0.0619(2) 0.3795(2) 0.38085(14) 0.0772(9) Uani 1 1 d . . . S2 S -0.2551(2) 0.4096(2) 0.23264(14) 0.0777(9) Uani 1 1 d . . . O1 O 0.0081(6) 0.1740(5) 0.2884(3) 0.069(2) Uani 1 1 d . . . O2 O -0.0338(5) 0.1999(5) 0.1848(3) 0.0645(19) Uani 1 1 d . . . O3 O 0.1120(7) 0.3462(6) 0.2107(3) 0.086(2) Uani 1 1 d . . . O4 O 0.0409(7) 0.4565(8) 0.1379(5) 0.120(4) Uani 1 1 d . . . N1 N 0.4592(8) 0.3390(7) 0.4396(4) 0.077(3) Uani 1 1 d . . . H1N H 0.4119 0.3318 0.4138 0.092 Uiso 1 1 calc R . . N2 N 0.2094(6) 0.3615(6) 0.4662(4) 0.062(2) Uani 1 1 d . . . N3 N 0.0982(6) 0.3689(6) 0.4555(4) 0.062(2) Uani 1 1 d . . . H3N H 0.0433 0.3785 0.4886 0.075 Uiso 1 1 calc R . . N4 N 0.1644(7) 0.3390(6) 0.3445(4) 0.071(3) Uani 1 1 d . . . H4A H 0.2324 0.3300 0.3539 0.085 Uiso 1 1 calc R . . H4B H 0.1529 0.3336 0.3036 0.085 Uiso 1 1 calc R . . N5 N -0.2332(8) 0.3359(7) -0.0860(4) 0.081(3) Uani 1 1 d . . . H5N H -0.2003 0.3396 -0.0514 0.097 Uiso 1 1 calc R . . N6 N -0.3298(6) 0.3776(6) 0.0531(4) 0.060(2) Uani 1 1 d . . . N7 N -0.3340(6) 0.3876(6) 0.1229(4) 0.060(2) Uani 1 1 d . . . H7N H -0.3952 0.3856 0.1506 0.072 Uiso 1 1 calc R . . N8 N -0.1507(7) 0.4056(7) 0.1036(4) 0.083(3) Uani 1 1 d . . . H8A H -0.1484 0.4009 0.0606 0.100 Uiso 1 1 calc R . . H8B H -0.0920 0.4139 0.1190 0.100 Uiso 1 1 calc R . . C1 C 0.5750(10) 0.3274(11) 0.4207(7) 0.099(4) Uani 1 1 d . . . H1 H 0.6139 0.3111 0.3781 0.119 Uiso 1 1 calc R . . C2 C 0.6226(11) 0.3435(10) 0.4739(7) 0.097(4) Uani 1 1 d . . . H2 H 0.6994 0.3402 0.4743 0.116 Uiso 1 1 calc R . . C3 C 0.5356(11) 0.3664(10) 0.5285(7) 0.087(4) Uani 1 1 d . . . C4 C 0.5284(12) 0.3854(11) 0.5966(7) 0.102(5) Uani 1 1 d . . . H4 H 0.5947 0.3837 0.6147 0.122 Uiso 1 1 calc R . . C5 C 0.4278(12) 0.4063(12) 0.6369(7) 0.112(6) Uani 1 1 d . . . H5 H 0.4258 0.4216 0.6814 0.135 Uiso 1 1 calc R . . C6 C 0.3260(11) 0.4053(9) 0.6131(6) 0.093(4) Uani 1 1 d . . . H6 H 0.2578 0.4198 0.6420 0.111 Uiso 1 1 calc R . . C7 C 0.3258(9) 0.3832(8) 0.5476(5) 0.065(3) Uani 1 1 d . . . C8 C 0.4311(10) 0.3639(8) 0.5069(6) 0.069(3) Uani 1 1 d . . . C9 C 0.2171(9) 0.3840(8) 0.5259(5) 0.066(3) Uani 1 1 d . . . H9 H 0.1511 0.4013 0.5562 0.079 Uiso 1 1 calc R . . C10 C 0.0789(8) 0.3607(8) 0.3920(5) 0.060(3) Uani 1 1 d . . . C11 C -0.1809(14) 0.3218(10) -0.1520(7) 0.112(5) Uani 1 1 d . . . H11 H -0.1037 0.3165 -0.1664 0.134 Uiso 1 1 calc R . . C12 C -0.2574(18) 0.3170(11) -0.1927(7) 0.124(6) Uani 1 1 d . . . H12 H -0.2418 0.3065 -0.2389 0.148 Uiso 1 1 calc R . . C13 C -0.3661(15) 0.3307(10) -0.1526(7) 0.092(4) Uani 1 1 d . . . C14 C -0.4733(18) 0.3340(11) -0.1652(8) 0.119(6) Uani 1 1 d . . . H14 H -0.4852 0.3252 -0.2090 0.142 Uiso 1 1 calc R . . C15 C -0.5639(15) 0.3501(11) -0.1145(7) 0.109(5) Uani 1 1 d . . . H15 H -0.6372 0.3531 -0.1232 0.131 Uiso 1 1 calc R . . C16 C -0.5428(12) 0.3619(10) -0.0494(6) 0.096(4) Uani 1 1 d . . . H16 H -0.6046 0.3732 -0.0152 0.116 Uiso 1 1 calc R . . C17 C -0.4380(9) 0.3579(8) -0.0323(5) 0.065(3) Uani 1 1 d . . . C18 C -0.3485(10) 0.3431(7) -0.0855(5) 0.063(3) Uani 1 1 d . . . C19 C -0.4248(8) 0.3715(8) 0.0363(5) 0.066(3) Uani 1 1 d . . . H19 H -0.4877 0.3760 0.0699 0.079 Uiso 1 1 calc R . . C20 C -0.2438(8) 0.4002(7) 0.1458(5) 0.057(3) Uani 1 1 d . . . C21 C 0.0025(8) 0.1476(7) 0.2336(5) 0.052(3) Uani 1 1 d . . . C22 C 0.0475(12) 0.0427(10) 0.2191(6) 0.104(5) Uani 1 1 d . . . H22A H 0.1277 0.0316 0.2045 0.157 Uiso 1 1 calc R . . H22B H 0.0104 0.0278 0.1838 0.157 Uiso 1 1 calc R . . H22C H 0.0321 0.0037 0.2600 0.157 Uiso 1 1 calc R . . C23 C 0.1230(8) 0.4048(9) 0.1617(5) 0.066(3) Uani 1 1 d . . . C24 C 0.2382(10) 0.4148(10) 0.1295(6) 0.096(4) Uani 1 1 d . . . H24A H 0.2926 0.3825 0.1584 0.144 Uiso 1 1 calc R . . H24B H 0.2411 0.4802 0.1233 0.144 Uiso 1 1 calc R . . H24C H 0.2553 0.3883 0.0859 0.144 Uiso 1 1 calc R . . Cd2 Cd 0.49173(6) 0.16613(6) 0.23805(4) 0.0623(3) Uani 1 1 d . . . S3 S 0.3251(3) 0.0889(3) 0.26527(14) 0.0790(9) Uani 1 1 d . . . S4 S 0.5761(2) 0.1205(2) 0.11560(14) 0.0738(8) Uani 1 1 d . . . O5 O 0.4870(5) 0.3243(5) 0.2074(3) 0.0630(19) Uani 1 1 d . . . O6 O 0.4048(5) 0.2988(5) 0.3109(3) 0.069(2) Uani 1 1 d . . . O7 O 0.6466(6) 0.1512(6) 0.2868(3) 0.083(2) Uani 1 1 d . . . O8 O 0.5963(7) 0.0445(8) 0.3604(5) 0.115(4) Uani 1 1 d . . . N9 N 0.1260(8) 0.1637(7) 0.5851(4) 0.076(3) Uani 1 1 d . . . H9A H 0.1801 0.1603 0.5514 0.091 Uiso 1 1 calc R . . N10 N 0.1342(7) 0.1209(6) 0.4433(4) 0.058(2) Uani 1 1 d . . . N11 N 0.1747(7) 0.1124(6) 0.3736(4) 0.058(2) Uani 1 1 d . . . H11N H 0.1276 0.1151 0.3452 0.070 Uiso 1 1 calc R . . N12 N 0.3566(7) 0.0934(7) 0.3942(4) 0.081(3) Uani 1 1 d . . . H12A H 0.3322 0.0969 0.4371 0.097 Uiso 1 1 calc R . . H12B H 0.4280 0.0855 0.3800 0.097 Uiso 1 1 calc R . . N13 N 1.1050(7) 0.1648(7) 0.0543(4) 0.070(3) Uani 1 1 d . . . H13N H 1.0419 0.1671 0.0810 0.084 Uiso 1 1 calc R . . N14 N 0.8838(6) 0.1339(6) 0.0301(4) 0.054(2) Uani 1 1 d . . . N15 N 0.7710(7) 0.1246(6) 0.0421(4) 0.064(2) Uani 1 1 d . . . H15N H 0.7394 0.1118 0.0095 0.077 Uiso 1 1 calc R . . N16 N 0.7628(7) 0.1584(6) 0.1523(4) 0.067(2) Uani 1 1 d . . . H16A H 0.8316 0.1659 0.1429 0.080 Uiso 1 1 calc R . . H16B H 0.7269 0.1659 0.1929 0.080 Uiso 1 1 calc R . . C25 C 0.1335(13) 0.1818(10) 0.6511(6) 0.101(5) Uani 1 1 d . . . H25 H 0.1977 0.1923 0.6661 0.121 Uiso 1 1 calc R . . C26 C 0.0333(14) 0.1817(10) 0.6900(7) 0.099(4) Uani 1 1 d . . . H26 H 0.0163 0.1922 0.7362 0.118 Uiso 1 1 calc R . . C27 C -0.0416(12) 0.1633(9) 0.6492(6) 0.082(4) Uani 1 1 d . . . C28 C -0.1554(12) 0.1544(10) 0.6602(7) 0.096(4) Uani 1 1 d . . . H28 H -0.1967 0.1598 0.7036 0.115 Uiso 1 1 calc R . . C29 C -0.2067(13) 0.1376(11) 0.6061(7) 0.107(5) Uani 1 1 d . . . H29 H -0.2821 0.1322 0.6132 0.128 Uiso 1 1 calc R . . C30 C -0.1436(9) 0.1292(9) 0.5417(6) 0.080(4) Uani 1 1 d . . . H30 H -0.1792 0.1188 0.5060 0.096 Uiso 1 1 calc R . . C31 C -0.0335(9) 0.1351(7) 0.5277(5) 0.061(3) Uani 1 1 d . . . C32 C 0.0198(9) 0.1521(8) 0.5820(5) 0.065(3) Uani 1 1 d . . . C33 C 0.0286(9) 0.1250(8) 0.4589(5) 0.069(3) Uani 1 1 d . . . H33 H -0.0123 0.1214 0.4239 0.083 Uiso 1 1 calc R . . C34 C 0.2853(8) 0.1001(8) 0.3508(5) 0.065(3) Uani 1 1 d . . . C35 C 1.2022(10) 0.1802(10) 0.0719(6) 0.086(4) Uani 1 1 d . . . H35 H 1.2106 0.1934 0.1153 0.103 Uiso 1 1 calc R . . C36 C 1.2841(10) 0.1737(10) 0.0180(6) 0.089(4) Uani 1 1 d . . . H36 H 1.3573 0.1825 0.0173 0.107 Uiso 1 1 calc R . . C37 C 1.2384(10) 0.1509(9) -0.0376(6) 0.075(3) Uani 1 1 d . . . C38 C 1.2785(10) 0.1339(10) -0.1059(6) 0.088(4) Uani 1 1 d . . . H38 H 1.3525 0.1375 -0.1239 0.105 Uiso 1 1 calc R . . C39 C 1.2086(10) 0.1118(9) -0.1464(6) 0.085(4) Uani 1 1 d . . . H39 H 1.2364 0.0990 -0.1916 0.102 Uiso 1 1 calc R . . C40 C 1.0957(10) 0.1083(8) -0.1208(5) 0.075(3) Uani 1 1 d . . . H40 H 1.0498 0.0943 -0.1497 0.089 Uiso 1 1 calc R . . C41 C 1.0509(8) 0.1250(7) -0.0542(5) 0.060(3) Uani 1 1 d . . . C42 C 1.1245(9) 0.1449(8) -0.0127(5) 0.063(3) Uani 1 1 d . . . C43 C 0.9342(9) 0.1194(8) -0.0303(5) 0.067(3) Uani 1 1 d . . . H43 H 0.8929 0.1041 -0.0614 0.080 Uiso 1 1 calc R . . C44 C 0.7126(8) 0.1356(7) 0.1045(5) 0.057(3) Uani 1 1 d . . . C45 C 0.4366(9) 0.3498(7) 0.2632(4) 0.052(3) Uani 1 1 d . . . C46 C 0.4110(10) 0.4534(9) 0.2754(7) 0.094(4) Uani 1 1 d . . . H46A H 0.3305 0.4765 0.2828 0.142 Uiso 1 1 calc R . . H46B H 0.4436 0.4875 0.2362 0.142 Uiso 1 1 calc R . . H46C H 0.4429 0.4619 0.3148 0.142 Uiso 1 1 calc R . . C47 C 0.6614(8) 0.0924(9) 0.3367(5) 0.066(3) Uani 1 1 d . . . C48 C 0.7658(10) 0.0833(11) 0.3670(6) 0.108(5) Uani 1 1 d . . . H48A H 0.7662 0.0381 0.4056 0.161 Uiso 1 1 calc R . . H48B H 0.7692 0.1430 0.3814 0.161 Uiso 1 1 calc R . . H48C H 0.8303 0.0629 0.3336 0.161 Uiso 1 1 calc R . . O9 O 0.6303(8) -0.1012(8) 0.4605(5) 0.111(3) Uani 1 1 d . . . H9B H 0.6279 -0.0511 0.4375 0.166 Uiso 1 1 calc R . . C49 C 0.5250(18) -0.1293(13) 0.4646(10) 0.167(8) Uani 1 1 d . . . H49A H 0.5228 -0.1816 0.4978 0.251 Uiso 1 1 calc R . . H49B H 0.5173 -0.1472 0.4207 0.251 Uiso 1 1 calc R . . H49C H 0.4640 -0.0779 0.4779 0.251 Uiso 1 1 calc R . . O10 O 0.0504(8) 0.5990(9) 0.0401(5) 0.124(4) Uani 1 1 d . . . H10 H 0.0616 0.5564 0.0701 0.186 Uiso 1 1 calc R . . C50 C -0.057(2) 0.6248(17) 0.0373(14) 0.253(14) Uani 1 1 d . . . H50A H -0.0812 0.5785 0.0161 0.379 Uiso 1 1 calc R . . H50B H -0.0715 0.6839 0.0109 0.379 Uiso 1 1 calc R . . H50C H -0.0967 0.6313 0.0827 0.379 Uiso 1 1 calc R . . O11 O -0.0579(13) 0.3990(11) 0.5752(7) 0.182(6) Uani 1 1 d . . . H11A H -0.0363 0.3969 0.6125 0.273 Uiso 1 1 calc RD . . C51 C -0.1736(16) 0.3942(16) 0.5850(15) 0.243(14) Uani 1 1 d . . . H51A H -0.2175 0.4462 0.6096 0.364 Uiso 1 1 calc RD . . H51B H -0.1831 0.3364 0.6105 0.364 Uiso 1 1 calc RD . . H51C H -0.1989 0.3966 0.5413 0.364 Uiso 1 1 calc R . . O12 O 0.7036(10) 0.0571(10) -0.0698(6) 0.158(5) Uani 1 1 d . . . H12C H 0.7277 0.0003 -0.0714 0.237 Uiso 1 1 calc RD . . C52 C 0.6125(17) 0.0809(14) -0.0961(11) 0.188(10) Uani 1 1 d . . . H52A H 0.6043 0.1447 -0.1152 0.282 Uiso 1 1 calc R . . H52B H 0.5493 0.0756 -0.0615 0.282 Uiso 1 1 calc RD . . H52C H 0.6150 0.0404 -0.1315 0.282 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 Cd1 0.0562(5) 0.0876(6) 0.0580(5) -0.0021(4) -0.0176(4) -0.0176(4) S1 0.0447(15) 0.123(3) 0.0626(16) -0.0242(16) -0.0071(13) -0.0083(15) S2 0.0529(16) 0.120(3) 0.0615(16) -0.0115(16) -0.0165(14) -0.0125(16) O1 0.073(5) 0.101(6) 0.044(4) 0.002(4) -0.019(4) -0.034(4) O2 0.064(4) 0.083(5) 0.054(4) -0.002(3) -0.016(3) -0.028(4) O3 0.099(6) 0.123(7) 0.044(4) 0.014(4) -0.004(4) -0.052(5) O4 0.056(5) 0.178(10) 0.130(7) 0.045(7) -0.024(5) -0.052(6) N1 0.068(6) 0.106(8) 0.059(6) -0.012(5) -0.015(5) -0.015(5) N2 0.052(5) 0.075(6) 0.062(5) -0.011(4) -0.015(4) -0.010(4) N3 0.046(5) 0.095(7) 0.050(5) -0.009(4) -0.007(4) -0.022(4) N4 0.048(5) 0.116(8) 0.050(5) -0.009(5) -0.018(5) -0.011(5) N5 0.086(7) 0.096(8) 0.052(6) 0.002(5) 0.006(5) -0.016(6) N6 0.043(4) 0.083(6) 0.047(5) 0.006(4) -0.006(4) -0.008(4) N7 0.038(4) 0.093(7) 0.048(5) -0.005(4) -0.003(4) -0.015(4) N8 0.060(6) 0.147(10) 0.045(5) 0.024(5) -0.013(5) -0.038(6) C1 0.062(8) 0.145(13) 0.090(9) -0.011(8) -0.016(7) -0.014(8) C2 0.059(8) 0.137(13) 0.102(10) -0.012(9) -0.030(8) -0.021(8) C3 0.075(8) 0.104(10) 0.091(9) -0.030(7) -0.031(8) -0.012(7) C4 0.076(9) 0.136(13) 0.102(10) -0.036(9) -0.037(9) -0.010(8) C5 0.083(10) 0.172(16) 0.097(10) -0.066(10) -0.039(9) -0.014(10) C6 0.097(9) 0.108(11) 0.083(8) -0.032(7) -0.037(8) -0.014(8) C7 0.067(7) 0.074(8) 0.053(6) -0.017(5) -0.016(6) -0.003(6) C8 0.070(8) 0.071(8) 0.069(7) -0.013(6) -0.022(7) -0.008(6) C9 0.057(6) 0.087(8) 0.055(6) -0.006(5) -0.008(5) -0.018(6) C10 0.044(6) 0.083(8) 0.050(6) -0.010(5) -0.002(5) -0.008(5) C11 0.123(13) 0.113(12) 0.078(10) -0.003(8) 0.017(9) -0.001(9) C12 0.186(19) 0.114(13) 0.066(9) -0.024(8) -0.010(12) -0.020(12) C13 0.121(12) 0.089(10) 0.065(8) 0.010(7) 0.004(9) -0.038(9) C14 0.175(17) 0.122(13) 0.081(10) 0.016(9) -0.062(12) -0.057(12) C15 0.142(14) 0.133(13) 0.074(9) 0.020(9) -0.049(10) -0.062(11) C16 0.109(10) 0.112(11) 0.083(8) 0.019(7) -0.039(8) -0.049(8) C17 0.060(7) 0.086(8) 0.050(6) -0.002(5) -0.003(6) -0.020(6) C18 0.078(8) 0.056(7) 0.057(7) 0.012(5) -0.012(6) -0.022(6) C19 0.050(6) 0.094(9) 0.057(6) 0.014(5) -0.014(5) -0.026(6) C20 0.045(6) 0.071(7) 0.051(6) 0.012(5) -0.006(5) -0.008(5) C21 0.055(6) 0.059(7) 0.041(5) 0.009(5) -0.001(5) -0.020(5) C22 0.129(12) 0.111(12) 0.083(8) 0.002(8) -0.046(9) -0.029(9) C23 0.047(6) 0.105(9) 0.055(6) -0.012(6) -0.009(5) -0.027(6) C24 0.065(8) 0.124(12) 0.101(9) 0.015(8) -0.013(7) -0.036(7) Cd2 0.0496(4) 0.0793(6) 0.0570(5) -0.0008(4) -0.0011(4) -0.0182(4) S3 0.0700(18) 0.118(3) 0.0603(16) -0.0096(16) -0.0011(15) -0.0479(18) S4 0.0467(15) 0.111(3) 0.0706(17) -0.0234(16) -0.0002(13) -0.0291(15) O5 0.042(4) 0.084(5) 0.059(4) -0.005(4) -0.001(3) -0.009(3) O6 0.059(4) 0.097(6) 0.049(4) -0.009(4) 0.004(3) -0.021(4) O7 0.070(5) 0.129(7) 0.041(4) 0.024(4) -0.008(3) -0.018(4) O8 0.059(5) 0.154(9) 0.130(7) 0.059(7) -0.033(5) -0.036(6) N9 0.077(7) 0.097(8) 0.057(5) -0.004(5) -0.011(5) -0.023(5) N10 0.057(5) 0.070(6) 0.044(5) 0.005(4) -0.008(4) -0.012(4) N11 0.053(5) 0.081(6) 0.047(5) 0.000(4) -0.014(4) -0.027(4) N12 0.048(5) 0.146(9) 0.048(5) 0.009(5) -0.002(4) -0.028(5) N13 0.065(6) 0.101(8) 0.050(5) -0.018(5) 0.002(4) -0.031(5) N14 0.049(5) 0.074(6) 0.044(5) -0.006(4) -0.005(4) -0.027(4) N15 0.050(5) 0.097(7) 0.055(5) -0.006(5) -0.009(4) -0.034(5) N16 0.052(5) 0.109(8) 0.045(4) -0.014(4) 0.001(4) -0.029(5) C25 0.106(11) 0.136(13) 0.063(8) -0.021(8) -0.024(8) -0.014(9) C26 0.124(12) 0.109(11) 0.063(8) -0.016(7) -0.016(9) -0.019(9) C27 0.096(10) 0.083(9) 0.061(7) 0.007(6) -0.012(7) -0.014(7) C28 0.085(10) 0.109(11) 0.078(9) 0.000(7) 0.026(8) -0.014(8) C29 0.089(10) 0.131(13) 0.093(10) 0.015(9) 0.002(9) -0.027(9) C30 0.058(7) 0.111(11) 0.071(8) 0.006(7) -0.001(6) -0.030(7) C31 0.070(7) 0.067(7) 0.046(6) 0.005(5) -0.003(5) -0.020(6) C32 0.068(7) 0.073(8) 0.046(6) 0.007(5) 0.004(5) -0.013(6) C33 0.060(7) 0.086(8) 0.052(6) -0.001(5) 0.000(5) -0.004(6) C34 0.052(6) 0.087(8) 0.059(6) 0.014(5) -0.010(5) -0.028(5) C35 0.064(7) 0.124(12) 0.081(8) -0.034(7) -0.018(7) -0.027(7) C36 0.062(7) 0.139(13) 0.079(8) -0.025(8) -0.003(7) -0.045(8) C37 0.071(8) 0.081(9) 0.074(8) -0.018(6) 0.022(6) -0.038(6) C38 0.063(7) 0.117(11) 0.078(8) -0.009(7) 0.015(7) -0.025(7) C39 0.073(8) 0.109(11) 0.071(7) -0.009(7) 0.004(7) -0.026(7) C40 0.075(8) 0.098(10) 0.053(7) -0.007(6) 0.002(6) -0.029(7) C41 0.059(6) 0.072(8) 0.051(6) 0.010(5) -0.005(5) -0.026(5) C42 0.066(7) 0.071(8) 0.053(6) -0.001(5) 0.000(5) -0.023(6) C43 0.065(7) 0.085(8) 0.060(7) -0.014(6) -0.014(6) -0.027(6) C44 0.049(6) 0.061(7) 0.061(6) 0.001(5) -0.008(5) -0.017(5) C45 0.067(6) 0.065(7) 0.022(5) 0.001(5) -0.005(5) -0.015(5) C46 0.084(9) 0.087(10) 0.115(10) -0.001(8) -0.021(8) -0.019(7) C47 0.034(5) 0.101(9) 0.061(7) 0.000(6) 0.002(5) -0.017(6) C48 0.070(8) 0.159(14) 0.098(9) 0.013(9) -0.035(8) -0.027(8) O9 0.086(6) 0.159(10) 0.091(6) 0.037(6) -0.031(5) -0.041(6) C49 0.20(2) 0.132(17) 0.168(17) 0.030(13) -0.067(17) -0.028(15) O10 0.072(6) 0.192(12) 0.095(7) 0.045(7) -0.011(5) -0.026(6) C50 0.25(3) 0.17(3) 0.31(4) 0.03(2) -0.07(3) 0.01(2) O11 0.155(12) 0.168(13) 0.196(13) -0.010(11) 0.035(11) -0.021(10) C51 0.17(2) 0.15(2) 0.39(4) 0.08(2) -0.03(3) -0.049(18) O12 0.109(8) 0.246(15) 0.146(9) -0.072(10) -0.049(8) -0.044(9) C52 0.181(19) 0.17(2) 0.23(2) 0.006(16) -0.136(19) -0.012(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 Cd1 O3 2.219(8) . Y Cd1 O1 2.319(8) . Y Cd1 O2 2.488(7) . Y Cd1 S2 2.510(3) . Y Cd1 S1 2.583(3) . Y S1 C10 1.727(10) . Y S2 C20 1.727(10) . Y O1 C21 1.209(11) . Y O2 C21 1.247(9) . Y O3 C23 1.240(12) . Y O4 C23 1.241(12) . Y N1 C1 1.382(15) . ? N1 C8 1.393(13) . ? N2 C9 1.287(12) . Y N2 N3 1.388(10) . Y N3 C10 1.342(11) . Y N4 C10 1.299(11) . Y N5 C11 1.381(15) . ? N5 C18 1.388(14) . ? N6 C19 1.282(11) . Y N6 N7 1.403(10) . Y N7 C20 1.312(11) . Y N8 C20 1.315(12) . Y C1 C2 1.351(16) . ? C2 C3 1.405(17) . ? C3 C4 1.395(17) . ? C3 C8 1.420(15) . ? C4 C5 1.349(18) . ? C5 C6 1.402(15) . ? C6 C7 1.375(14) . ? C7 C8 1.396(15) . ? C7 C9 1.457(13) . ? C11 C12 1.35(2) . ? C12 C13 1.42(2) . ? C13 C14 1.36(2) . ? C13 C18 1.420(16) . ? C14 C15 1.37(2) . ? C15 C16 1.393(16) . ? C16 C17 1.364(15) . ? C17 C18 1.391(14) . ? C17 C19 1.437(13) . ? C21 C22 1.554(16) . ? C23 C24 1.483(15) . ? Cd2 O7 2.219(7) . ? Cd2 O5 2.322(7) . ? Cd2 O6 2.487(7) . ? Cd2 S3 2.503(3) . ? Cd2 S4 2.583(3) . ? S3 C34 1.707(10) . ? S4 C44 1.708(10) . ? O5 C45 1.231(10) . ? O6 C45 1.213(11) . ? O7 C47 1.250(12) . ? O8 C47 1.187(13) . ? N9 C32 1.358(13) . ? N9 C25 1.388(13) . ? N10 C33 1.268(12) . ? N10 N11 1.404(10) . ? N11 C34 1.334(12) . ? N12 C34 1.301(11) . ? N13 C35 1.359(12) . ? N13 C42 1.366(12) . ? N14 C43 1.275(12) . ? N14 N15 1.397(10) . ? N15 C44 1.337(12) . ? N16 C44 1.317(11) . ? C25 C26 1.341(18) . ? C26 C27 1.399(17) . ? C27 C28 1.407(17) . ? C27 C32 1.431(15) . ? C28 C29 1.394(18) . ? C29 C30 1.389(17) . ? C30 C31 1.350(14) . ? C31 C32 1.416(14) . ? C31 C33 1.458(14) . ? C35 C36 1.340(16) . ? C36 C37 1.414(15) . ? C37 C38 1.396(15) . ? C37 C42 1.421(15) . ? C38 C39 1.372(16) . ? C39 C40 1.403(16) . ? C40 C41 1.376(14) . ? C41 C42 1.406(14) . ? C41 C43 1.447(14) . ? C45 C46 1.517(15) . ? C47 C48 1.469(13) . ? O9 C49 1.42(2) . ? O10 C50 1.29(2) . ? O11 C51 1.41(3) . ? O12 C52 1.267(16) . ? 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 O3 Cd1 O1 90.2(3) . . Y O3 Cd1 O2 85.6(3) . . Y O1 Cd1 O2 53.6(2) . . Y O3 Cd1 S2 132.8(2) . . Y O1 Cd1 S2 127.99(19) . . Y O2 Cd1 S2 95.76(16) . . Y O3 Cd1 S1 101.0(2) . . Y O1 Cd1 S1 93.07(18) . . Y O2 Cd1 S1 146.33(16) . . Y S2 Cd1 S1 103.07(10) . . Y C10 S1 Cd1 105.4(4) . . Y C20 S2 Cd1 103.0(3) . . Y C21 O1 Cd1 95.3(5) . . ? C21 O2 Cd1 86.5(6) . . ? C23 O3 Cd1 119.5(7) . . ? C1 N1 C8 109.4(9) . . ? C9 N2 N3 112.9(8) . . ? C10 N3 N2 118.0(8) . . ? C11 N5 C18 107.5(11) . . ? C19 N6 N7 113.8(8) . . ? C20 N7 N6 119.6(8) . . ? C2 C1 N1 109.2(12) . . ? C1 C2 C3 107.8(11) . . ? C4 C3 C2 136.4(12) . . ? C4 C3 C8 115.3(13) . . ? C2 C3 C8 108.3(10) . . ? C5 C4 C3 121.6(11) . . ? C4 C5 C6 121.4(12) . . ? C7 C6 C5 120.8(13) . . ? C6 C7 C8 116.3(10) . . ? C6 C7 C9 118.2(11) . . ? C8 C7 C9 125.5(9) . . ? N1 C8 C7 130.2(9) . . ? N1 C8 C3 105.3(11) . . ? C7 C8 C3 124.5(10) . . ? N2 C9 C7 122.2(10) . . ? N4 C10 N3 119.3(8) . . ? N4 C10 S1 125.1(7) . . ? N3 C10 S1 115.6(8) . . ? C12 C11 N5 110.5(15) . . ? C11 C12 C13 108.0(13) . . ? C14 C13 C18 119.2(14) . . ? C14 C13 C12 134.8(15) . . ? C18 C13 C12 106.1(13) . . ? C13 C14 C15 121.0(13) . . ? C14 C15 C16 117.9(14) . . ? C17 C16 C15 124.7(14) . . ? C16 C17 C18 115.7(10) . . ? C16 C17 C19 120.6(11) . . ? C18 C17 C19 123.7(9) . . ? N5 C18 C17 130.5(9) . . ? N5 C18 C13 107.9(11) . . ? C17 C18 C13 121.5(11) . . ? N6 C19 C17 122.7(10) . . ? N7 C20 N8 120.6(9) . . ? N7 C20 S2 116.7(8) . . ? N8 C20 S2 122.7(8) . . ? O1 C21 O2 124.5(10) . . ? O1 C21 C22 120.2(8) . . ? O2 C21 C22 115.2(9) . . ? O4 C23 O3 122.8(10) . . ? O4 C23 C24 117.7(10) . . ? O3 C23 C24 119.6(9) . . ? O7 Cd2 O5 91.8(3) . . ? O7 Cd2 O6 87.1(3) . . ? O5 Cd2 O6 53.6(2) . . ? O7 Cd2 S3 132.4(2) . . ? O5 Cd2 S3 126.68(17) . . ? O6 Cd2 S3 94.50(19) . . ? O7 Cd2 S4 101.9(2) . . ? O5 Cd2 S4 92.1(2) . . ? O6 Cd2 S4 145.07(18) . . ? S3 Cd2 S4 103.30(10) . . ? C34 S3 Cd2 103.4(4) . . ? C44 S4 Cd2 105.6(4) . . ? C45 O5 Cd2 94.1(6) . . ? C45 O6 Cd2 86.7(6) . . ? C47 O7 Cd2 118.6(7) . . ? C32 N9 C25 109.3(10) . . ? C33 N10 N11 114.5(8) . . ? C34 N11 N10 120.9(7) . . ? C35 N13 C42 108.6(9) . . ? C43 N14 N15 115.3(8) . . ? C44 N15 N14 119.4(8) . . ? C26 C25 N9 109.0(13) . . ? C25 C26 C27 108.5(12) . . ? C26 C27 C28 135.1(13) . . ? C26 C27 C32 106.8(12) . . ? C28 C27 C32 118.1(11) . . ? C29 C28 C27 120.3(12) . . ? C30 C29 C28 119.1(13) . . ? C31 C30 C29 123.9(12) . . ? C30 C31 C32 117.8(10) . . ? C30 C31 C33 121.4(10) . . ? C32 C31 C33 120.9(10) . . ? N9 C32 C31 132.6(10) . . ? N9 C32 C27 106.5(10) . . ? C31 C32 C27 120.9(10) . . ? N10 C33 C31 124.8(10) . . ? N12 C34 N11 119.3(9) . . ? N12 C34 S3 123.7(8) . . ? N11 C34 S3 116.9(7) . . ? C36 C35 N13 110.8(10) . . ? C35 C36 C37 107.2(10) . . ? C38 C37 C36 135.8(12) . . ? C38 C37 C42 117.8(11) . . ? C36 C37 C42 106.5(10) . . ? C39 C38 C37 120.0(11) . . ? C38 C39 C40 120.9(12) . . ? C41 C40 C39 121.9(11) . . ? C40 C41 C42 116.5(10) . . ? C40 C41 C43 119.5(10) . . ? C42 C41 C43 124.0(10) . . ? N13 C42 C41 130.1(10) . . ? N13 C42 C37 107.0(9) . . ? C41 C42 C37 122.9(10) . . ? N14 C43 C41 124.9(9) . . ? N16 C44 N15 118.4(9) . . ? N16 C44 S4 125.0(8) . . ? N15 C44 S4 116.6(7) . . ? O6 C45 O5 125.6(10) . . ? O6 C45 C46 115.5(10) . . ? O5 C45 C46 118.9(9) . . ? O8 C47 O7 123.8(9) . . ? O8 C47 C48 119.1(10) . . ? O7 C47 C48 117.2(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O6 0.86 2.17 2.891(10) 141.3 . N1 H1N N2 0.86 2.49 2.964(12) 115.6 . N3 H3N O11 0.86 1.96 2.811(16) 168.5 . N4 H4A O6 0.86 2.11 2.849(11) 143.5 . N4 H4B O3 0.86 1.97 2.816(10) 169.2 . N5 H5N O10 0.86 2.26 2.917(15) 132.7 2_565 N5 H5N N6 0.86 2.44 2.898(12) 114.3 . N7 H7N O5 0.86 2.00 2.807(10) 155.9 1_455 N8 H8A O10 0.86 2.16 2.925(13) 147.4 2_565 N8 H8B O4 0.86 1.97 2.810(12) 166.8 . N9 H9A O9 0.86 2.27 2.937(14) 134.7 2_656 N9 H9A N10 0.86 2.46 2.931(11) 115.2 . N11 H11N O1 0.86 1.98 2.789(9) 157.2 . N12 H12A O9 0.86 2.17 2.932(12) 148.3 2_656 N12 H12B O8 0.86 2.00 2.844(12) 168.4 . N13 H13N O2 0.86 2.18 2.891(11) 140.1 1_655 N13 H13N N14 0.86 2.48 2.959(11) 116.1 . N15 H15N O12 0.86 1.99 2.830(12) 165.0 . N16 H16A O2 0.86 2.13 2.869(10) 143.8 1_655 N16 H16B O7 0.86 1.98 2.823(10) 166.7 . O9 H9B O8 0.82 1.99 2.766(12) 158.4 . O10 H10 O4 0.82 1.91 2.706(13) 162.5 . _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.939 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.118 loop_ _shelx_res_file ; TITL [Cd(LH2)2(OAc)2] CELL 0.71073 12.2228 14.6495 19.8687 83.911 80.867 77.101 ZERR 4.00 0.0066 0.0092 0.0110 0.033 0.032 0.036 LATT 1 SFAC C H Cd N O S UNIT 104 136 4 32 24 8 omit 0 1 1 omit 1 1 1 OMIT -2 50.5 L.S. 12 dang -2.2 0.01 H11A H51A dang -2.2 0.01 H11A H51B DANG -2.2 0.01 H12C H52B acta SIZE 0.030 0.110 0.150 TEMP 23.000 WGHT 0.097600 FVAR 0.15916 CD1 3 -0.060378 0.331690 0.259179 11.00000 0.05624 0.08755 = 0.05797 -0.00213 -0.01765 -0.01760 S1 6 -0.061892 0.379501 0.380848 11.00000 0.04472 0.12344 = 0.06255 -0.02420 -0.00707 -0.00831 S2 6 -0.255073 0.409591 0.232640 11.00000 0.05293 0.11994 = 0.06153 -0.01154 -0.01647 -0.01249 O1 5 0.008127 0.174034 0.288364 11.00000 0.07262 0.10069 = 0.04406 0.00193 -0.01903 -0.03428 O2 5 -0.033849 0.199947 0.184783 11.00000 0.06413 0.08336 = 0.05383 -0.00153 -0.01585 -0.02811 O3 5 0.112050 0.346181 0.210736 11.00000 0.09929 0.12304 = 0.04391 0.01432 -0.00376 -0.05196 O4 5 0.040913 0.456477 0.137855 11.00000 0.05622 0.17825 = 0.12976 0.04477 -0.02387 -0.05230 N1 4 0.459235 0.338955 0.439574 11.00000 0.06781 0.10635 = 0.05881 -0.01208 -0.01502 -0.01519 AFIX 43 H1N 2 0.411925 0.331834 0.413807 11.00000 -1.20000 AFIX 0 N2 4 0.209428 0.361509 0.466212 11.00000 0.05176 0.07546 = 0.06224 -0.01053 -0.01533 -0.01041 N3 4 0.098183 0.368912 0.455482 11.00000 0.04640 0.09518 = 0.04954 -0.00869 -0.00690 -0.02200 AFIX 43 H3N 2 0.043257 0.378467 0.488554 11.00000 -1.20000 AFIX 0 N4 4 0.164369 0.339003 0.344470 11.00000 0.04801 0.11563 = 0.04992 -0.00944 -0.01796 -0.01092 AFIX 93 H4A 2 0.232435 0.330044 0.353867 11.00000 -1.20000 H4B 2 0.152924 0.333580 0.303612 11.00000 -1.20000 AFIX 0 N5 4 -0.233185 0.335921 -0.085963 11.00000 0.08619 0.09624 = 0.05155 0.00214 0.00573 -0.01611 AFIX 43 H5N 2 -0.200329 0.339557 -0.051432 11.00000 -1.20000 AFIX 0 N6 4 -0.329779 0.377587 0.053050 11.00000 0.04347 0.08340 = 0.04719 0.00595 -0.00588 -0.00761 N7 4 -0.333967 0.387627 0.122906 11.00000 0.03836 0.09278 = 0.04771 -0.00520 -0.00269 -0.01538 AFIX 43 H7N 2 -0.395232 0.385559 0.150563 11.00000 -1.20000 AFIX 0 N8 4 -0.150672 0.405622 0.103611 11.00000 0.05966 0.14685 = 0.04523 0.02388 -0.01329 -0.03798 AFIX 93 H8A 2 -0.148431 0.400933 0.060610 11.00000 -1.20000 H8B 2 -0.091968 0.413864 0.119031 11.00000 -1.20000 AFIX 0 C1 1 0.574979 0.327396 0.420698 11.00000 0.06193 0.14526 = 0.09004 -0.01144 -0.01637 -0.01375 AFIX 43 H1 2 0.613910 0.311075 0.378079 11.00000 -1.20000 AFIX 0 C2 1 0.622649 0.343547 0.473924 11.00000 0.05861 0.13697 = 0.10217 -0.01228 -0.03019 -0.02062 AFIX 43 H2 2 0.699433 0.340163 0.474336 11.00000 -1.20000 AFIX 0 C3 1 0.535616 0.366366 0.528546 11.00000 0.07497 0.10403 = 0.09083 -0.02990 -0.03140 -0.01173 C4 1 0.528444 0.385405 0.596620 11.00000 0.07590 0.13630 = 0.10184 -0.03646 -0.03732 -0.01021 AFIX 43 H4 2 0.594655 0.383665 0.614656 11.00000 -1.20000 AFIX 0 C5 1 0.427790 0.406274 0.636900 11.00000 0.08310 0.17225 = 0.09694 -0.06563 -0.03876 -0.01440 AFIX 43 H5 2 0.425835 0.421625 0.681371 11.00000 -1.20000 AFIX 0 C6 1 0.326012 0.405309 0.613123 11.00000 0.09699 0.10765 = 0.08335 -0.03215 -0.03684 -0.01416 AFIX 43 H6 2 0.257814 0.419785 0.642045 11.00000 -1.20000 AFIX 0 C7 1 0.325764 0.383239 0.547613 11.00000 0.06743 0.07410 = 0.05281 -0.01736 -0.01623 -0.00254 C8 1 0.431105 0.363946 0.506862 11.00000 0.06998 0.07124 = 0.06857 -0.01317 -0.02208 -0.00769 C9 1 0.217137 0.384002 0.525904 11.00000 0.05689 0.08677 = 0.05521 -0.00562 -0.00800 -0.01795 AFIX 43 H9 2 0.151126 0.401333 0.556217 11.00000 -1.20000 AFIX 0 C10 1 0.078872 0.360721 0.391977 11.00000 0.04371 0.08337 = 0.05016 -0.00997 -0.00168 -0.00809 C11 1 -0.180903 0.321846 -0.152042 11.00000 0.12274 0.11254 = 0.07824 -0.00305 0.01697 -0.00149 AFIX 43 H11 2 -0.103676 0.316459 -0.166442 11.00000 -1.20000 AFIX 0 C12 1 -0.257370 0.317012 -0.192711 11.00000 0.18644 0.11376 = 0.06608 -0.02395 -0.00955 -0.02019 AFIX 43 H12 2 -0.241781 0.306543 -0.238944 11.00000 -1.20000 AFIX 0 C13 1 -0.366083 0.330712 -0.152597 11.00000 0.12110 0.08906 = 0.06453 0.01029 0.00423 -0.03801 C14 1 -0.473280 0.334017 -0.165229 11.00000 0.17502 0.12224 = 0.08088 0.01572 -0.06162 -0.05749 AFIX 43 H14 2 -0.485157 0.325211 -0.208961 11.00000 -1.20000 AFIX 0 C15 1 -0.563899 0.350122 -0.114482 11.00000 0.14180 0.13321 = 0.07416 0.01952 -0.04938 -0.06227 AFIX 43 H15 2 -0.637197 0.353116 -0.123217 11.00000 -1.20000 AFIX 0 C16 1 -0.542797 0.361864 -0.049418 11.00000 0.10923 0.11203 = 0.08319 0.01893 -0.03945 -0.04929 AFIX 43 H16 2 -0.604561 0.373215 -0.015196 11.00000 -1.20000 AFIX 0 C17 1 -0.437954 0.357899 -0.032320 11.00000 0.05990 0.08561 = 0.04962 -0.00234 -0.00305 -0.01963 C18 1 -0.348460 0.343125 -0.085483 11.00000 0.07764 0.05617 = 0.05719 0.01210 -0.01159 -0.02165 C19 1 -0.424757 0.371452 0.036282 11.00000 0.04966 0.09415 = 0.05740 0.01370 -0.01382 -0.02578 AFIX 43 H19 2 -0.487677 0.375954 0.069869 11.00000 -1.20000 AFIX 0 C20 1 -0.243839 0.400189 0.145775 11.00000 0.04500 0.07060 = 0.05054 0.01191 -0.00552 -0.00811 C21 1 0.002501 0.147612 0.233627 11.00000 0.05463 0.05930 = 0.04071 0.00864 -0.00113 -0.01978 C22 1 0.047473 0.042658 0.219085 11.00000 0.12933 0.11118 = 0.08325 0.00169 -0.04610 -0.02947 AFIX 137 H22A 2 0.127745 0.031600 0.204504 11.00000 -1.50000 H22B 2 0.010392 0.027808 0.183797 11.00000 -1.50000 H22C 2 0.032056 0.003745 0.259975 11.00000 -1.50000 AFIX 0 C23 1 0.122957 0.404794 0.161701 11.00000 0.04675 0.10467 = 0.05498 -0.01182 -0.00895 -0.02675 C24 1 0.238159 0.414824 0.129473 11.00000 0.06486 0.12449 = 0.10127 0.01522 -0.01317 -0.03575 AFIX 137 H24A 2 0.292641 0.382471 0.158415 11.00000 -1.50000 H24B 2 0.241131 0.480156 0.123253 11.00000 -1.50000 H24C 2 0.255258 0.388335 0.085893 11.00000 -1.50000 AFIX 0 CD2 3 0.491731 0.166133 0.238053 11.00000 0.04959 0.07935 = 0.05705 -0.00076 -0.00107 -0.01819 S3 6 0.325145 0.088941 0.265266 11.00000 0.07004 0.11809 = 0.06035 -0.00961 -0.00107 -0.04793 S4 6 0.576065 0.120532 0.115599 11.00000 0.04673 0.11090 = 0.07063 -0.02343 -0.00019 -0.02906 O5 5 0.487014 0.324254 0.207390 11.00000 0.04161 0.08448 = 0.05851 -0.00452 -0.00061 -0.00908 O6 5 0.404830 0.298760 0.310888 11.00000 0.05931 0.09659 = 0.04933 -0.00931 0.00354 -0.02149 O7 5 0.646643 0.151247 0.286814 11.00000 0.06997 0.12856 = 0.04110 0.02385 -0.00774 -0.01813 O8 5 0.596272 0.044486 0.360399 11.00000 0.05886 0.15364 = 0.13014 0.05927 -0.03296 -0.03588 N9 4 0.126045 0.163683 0.585061 11.00000 0.07709 0.09686 = 0.05652 -0.00364 -0.01113 -0.02265 AFIX 43 H9A 2 0.180142 0.160317 0.551373 11.00000 -1.20000 AFIX 0 N10 4 0.134163 0.120895 0.443347 11.00000 0.05741 0.06990 = 0.04379 0.00489 -0.00849 -0.01202 N11 4 0.174714 0.112393 0.373629 11.00000 0.05347 0.08148 = 0.04706 -0.00002 -0.01430 -0.02694 AFIX 43 H11N 2 0.127596 0.115143 0.345233 11.00000 -1.20000 AFIX 0 N12 4 0.356556 0.093414 0.394181 11.00000 0.04819 0.14555 = 0.04806 0.00867 -0.00224 -0.02818 AFIX 93 H12A 2 0.332187 0.096914 0.437077 11.00000 -1.20000 H12B 2 0.428017 0.085488 0.379956 11.00000 -1.20000 AFIX 0 N13 4 1.105035 0.164768 0.054350 11.00000 0.06457 0.10136 = 0.05044 -0.01837 0.00231 -0.03135 AFIX 43 H13N 2 1.041903 0.167147 0.081023 11.00000 -1.20000 AFIX 0 N14 4 0.883812 0.133946 0.030070 11.00000 0.04935 0.07376 = 0.04435 -0.00565 -0.00469 -0.02747 N15 4 0.770990 0.124569 0.042064 11.00000 0.05025 0.09678 = 0.05535 -0.00588 -0.00933 -0.03372 AFIX 43 H15N 2 0.739370 0.111801 0.009525 11.00000 -1.20000 AFIX 0 N16 4 0.762823 0.158440 0.152320 11.00000 0.05188 0.10873 = 0.04495 -0.01410 0.00063 -0.02930 AFIX 93 H16A 2 0.831574 0.165878 0.142945 11.00000 -1.20000 H16B 2 0.726891 0.165912 0.192894 11.00000 -1.20000 AFIX 0 C25 1 0.133533 0.181805 0.651142 11.00000 0.10608 0.13597 = 0.06269 -0.02127 -0.02366 -0.01436 AFIX 43 H25 2 0.197727 0.192305 0.666080 11.00000 -1.20000 AFIX 0 C26 1 0.033261 0.181730 0.689973 11.00000 0.12425 0.10902 = 0.06330 -0.01577 -0.01640 -0.01881 AFIX 43 H26 2 0.016320 0.192163 0.736194 11.00000 -1.20000 AFIX 0 C27 1 -0.041565 0.163310 0.649222 11.00000 0.09622 0.08349 = 0.06107 0.00689 -0.01164 -0.01409 C28 1 -0.155433 0.154448 0.660167 11.00000 0.08455 0.10891 = 0.07762 -0.00022 0.02640 -0.01365 AFIX 43 H28 2 -0.196694 0.159826 0.703636 11.00000 -1.20000 AFIX 0 C29 1 -0.206691 0.137637 0.606128 11.00000 0.08861 0.13080 = 0.09341 0.01505 0.00232 -0.02740 AFIX 43 H29 2 -0.282082 0.132153 0.613163 11.00000 -1.20000 AFIX 0 C30 1 -0.143578 0.129200 0.541658 11.00000 0.05798 0.11075 = 0.07079 0.00596 -0.00066 -0.02973 AFIX 43 H30 2 -0.179240 0.118847 0.506012 11.00000 -1.20000 AFIX 0 C31 1 -0.033545 0.135133 0.527656 11.00000 0.07026 0.06693 = 0.04612 0.00451 -0.00318 -0.01998 C32 1 0.019816 0.152104 0.581979 11.00000 0.06783 0.07291 = 0.04556 0.00663 0.00369 -0.01261 C33 1 0.028568 0.125045 0.458921 11.00000 0.05967 0.08631 = 0.05151 -0.00084 -0.00004 -0.00370 AFIX 43 H33 2 -0.012275 0.121388 0.423948 11.00000 -1.20000 AFIX 0 C34 1 0.285329 0.100108 0.350818 11.00000 0.05214 0.08714 = 0.05852 0.01389 -0.00964 -0.02795 C35 1 1.202159 0.180152 0.071851 11.00000 0.06403 0.12445 = 0.08131 -0.03385 -0.01796 -0.02682 AFIX 43 H35 2 1.210578 0.193373 0.115272 11.00000 -1.20000 AFIX 0 C36 1 1.284132 0.173669 0.017996 11.00000 0.06223 0.13890 = 0.07941 -0.02491 -0.00347 -0.04509 AFIX 43 H36 2 1.357345 0.182473 0.017310 11.00000 -1.20000 AFIX 0 C37 1 1.238412 0.150931 -0.037587 11.00000 0.07082 0.08141 = 0.07417 -0.01796 0.02194 -0.03773 C38 1 1.278455 0.133884 -0.105879 11.00000 0.06309 0.11735 = 0.07802 -0.00908 0.01527 -0.02519 AFIX 43 H38 2 1.352528 0.137504 -0.123861 11.00000 -1.20000 AFIX 0 C39 1 1.208582 0.111801 -0.146449 11.00000 0.07341 0.10907 = 0.07060 -0.00905 0.00441 -0.02591 AFIX 43 H39 2 1.236412 0.098976 -0.191564 11.00000 -1.20000 AFIX 0 C40 1 1.095691 0.108291 -0.120835 11.00000 0.07463 0.09763 = 0.05309 -0.00746 0.00223 -0.02856 AFIX 43 H40 2 1.049839 0.094266 -0.149745 11.00000 -1.20000 AFIX 0 C41 1 1.050891 0.125006 -0.054163 11.00000 0.05873 0.07222 = 0.05090 0.00950 -0.00491 -0.02588 C42 1 1.124485 0.144894 -0.012702 11.00000 0.06564 0.07067 = 0.05305 -0.00138 0.00041 -0.02338 C43 1 0.934242 0.119413 -0.030338 11.00000 0.06517 0.08458 = 0.06040 -0.01350 -0.01393 -0.02738 AFIX 43 H43 2 0.892948 0.104073 -0.061394 11.00000 -1.20000 AFIX 0 C44 1 0.712570 0.135609 0.104548 11.00000 0.04903 0.06090 = 0.06088 0.00094 -0.00789 -0.01656 C45 1 0.436559 0.349841 0.263157 11.00000 0.06712 0.06503 = 0.02185 0.00094 -0.00485 -0.01472 C46 1 0.411050 0.453410 0.275363 11.00000 0.08380 0.08672 = 0.11471 -0.00133 -0.02103 -0.01949 AFIX 137 H46A 2 0.330479 0.476458 0.282805 11.00000 -1.50000 H46B 2 0.443601 0.487466 0.236164 11.00000 -1.50000 H46C 2 0.442925 0.461853 0.314846 11.00000 -1.50000 AFIX 0 C47 1 0.661375 0.092434 0.336707 11.00000 0.03433 0.10114 = 0.06102 0.00031 0.00201 -0.01699 C48 1 0.765804 0.083317 0.366955 11.00000 0.07015 0.15929 = 0.09757 0.01323 -0.03535 -0.02726 AFIX 137 H48A 2 0.766154 0.038102 0.405650 11.00000 -1.50000 H48B 2 0.769189 0.142998 0.381399 11.00000 -1.50000 H48C 2 0.830305 0.062895 0.333579 11.00000 -1.50000 AFIX 0 O9 5 0.630348 -0.101208 0.460533 11.00000 0.08591 0.15871 = 0.09095 0.03744 -0.03102 -0.04064 AFIX 147 H9B 2 0.627917 -0.051083 0.437526 11.00000 -1.50000 AFIX 0 C49 1 0.525019 -0.129265 0.464576 11.00000 0.20423 0.13170 = 0.16779 0.02973 -0.06707 -0.02842 AFIX 137 H49A 2 0.522780 -0.181625 0.497823 11.00000 -1.50000 H49B 2 0.517306 -0.147182 0.420750 11.00000 -1.50000 H49C 2 0.463987 -0.077897 0.477879 11.00000 -1.50000 AFIX 0 O10 5 0.050423 0.599016 0.040111 11.00000 0.07153 0.19184 = 0.09500 0.04476 -0.01080 -0.02580 AFIX 147 H10 2 0.061589 0.556398 0.070104 11.00000 -1.50000 AFIX 0 C50 1 -0.056526 0.624816 0.037282 11.00000 0.24808 0.17044 = 0.31301 0.02631 -0.07319 0.01462 AFIX 137 H50A 2 -0.081224 0.578458 0.016115 11.00000 -1.50000 H50B 2 -0.071460 0.683947 0.010916 11.00000 -1.50000 H50C 2 -0.096750 0.631306 0.082701 11.00000 -1.50000 AFIX 0 O11 5 -0.057883 0.399042 0.575216 11.00000 0.15520 0.16762 = 0.19575 -0.01048 0.03534 -0.02092 AFIX 147 H11A 2 -0.036289 0.396919 0.612483 11.00000 -1.50000 AFIX 0 C51 1 -0.173607 0.394173 0.584967 11.00000 0.17357 0.14945 = 0.38664 0.08393 -0.02889 -0.04887 AFIX 137 H51A 2 -0.217471 0.446177 0.609641 11.00000 -1.50000 H51B 2 -0.183057 0.336403 0.610545 11.00000 -1.50000 H51C 2 -0.198880 0.396633 0.541337 11.00000 -1.50000 AFIX 0 O12 5 0.703559 0.057059 -0.069806 11.00000 0.10887 0.24624 = 0.14615 -0.07226 -0.04908 -0.04364 AFIX 147 H12C 2 0.727703 0.000307 -0.071410 11.00000 -1.50000 AFIX 0 C52 1 0.612507 0.080890 -0.096112 11.00000 0.18104 0.16972 = 0.23339 0.00595 -0.13600 -0.01172 AFIX 137 H52A 2 0.604273 0.144671 -0.115169 11.00000 -1.50000 H52B 2 0.549287 0.075621 -0.061548 11.00000 -1.50000 H52C 2 0.614988 0.040430 -0.131545 11.00000 -1.50000 HKLF 4 REM sad in P-1 REM R1 = 0.0800 for 5254 Fo > 4sig(Fo) and 0.1902 for all 12116 data REM 787 parameters refined using 3 restraints END WGHT 0.0959 0.0000 REM Highest difference peak 0.939, deepest hole -0.843, 1-sigma level 0.118 Q1 1 0.0016 0.2757 0.2649 11.00000 0.05 0.94 Q2 1 0.5102 0.2202 0.2606 11.00000 0.05 0.81 Q3 1 0.2458 0.2203 0.2624 11.00000 0.05 0.75 Q4 1 -0.0352 0.3659 0.2275 11.00000 0.05 0.73 ; _database_code_depnum_ccdc_archive 'CCDC 939910' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[Pd(L)(LH2)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 N8 Pd S2' _chemical_formula_sum 'C20 H18 N8 Pd S2' _chemical_formula_weight 540.94 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.2138(2) _cell_length_b 11.6637(2) _cell_length_c 18.0652(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.385(3) _cell_angle_gamma 90.00 _cell_volume 2566.00(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9633 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.34 _exptl_crystal_description BLOCK _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7600 _exptl_absorpt_correction_T_max 0.8323 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18756 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5866 _reflns_number_gt 5136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. The crystal structure contains disordered solvent molecules which could not be satisfactorily modeled. The data were therefore treated with the SQUEEZE routine of PLATON. ; _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^)+(0.0364P)^2^+0.5236P] 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 5866 _refine_ls_number_parameters 289 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.002 _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 -0.046164(12) 0.318521(12) 0.532344(8) 0.02024(6) Uani 1 1 d . . . S1 S 0.00148(4) 0.40421(4) 0.64164(3) 0.02678(12) Uani 1 1 d . . . S2 S 0.05054(4) 0.16038(5) 0.57614(3) 0.02840(12) Uani 1 1 d . . . N1 N -0.09161(13) 0.24999(14) 0.43131(9) 0.0229(3) Uani 1 1 d . . . N2 N -0.14198(13) 0.45844(14) 0.51236(9) 0.0217(3) Uani 1 1 d . . . N3 N -0.13720(15) 0.54868(14) 0.56371(10) 0.0263(4) Uani 1 1 d . . . N4 N -0.07126(17) 0.60882(16) 0.67869(11) 0.0350(4) Uani 1 1 d . . . H4A H -0.1098 0.6723 0.6727 0.042 Uiso 1 1 calc R . . H4B H -0.0300 0.5973 0.7201 0.042 Uiso 1 1 calc R . . N5 N 0.46365(16) 0.02189(16) 0.38679(11) 0.0338(4) Uani 1 1 d . . . H5N H 0.4150 0.0719 0.4002 0.041 Uiso 1 1 calc R . . N6 N 0.28997(15) 0.00410(16) 0.48703(11) 0.0301(4) Uani 1 1 d . . . N7 N 0.20431(15) 0.03430(16) 0.52827(11) 0.0301(4) Uani 1 1 d D . . H7N H 0.1785(19) -0.0160(17) 0.5585(11) 0.036 Uiso 1 1 d D . . N8 N 0.19349(15) 0.21370(16) 0.47516(11) 0.0300(4) Uani 1 1 d D . . H8A H 0.1616(19) 0.2813(12) 0.4737(15) 0.036 Uiso 1 1 d D . . H8B H 0.2483(15) 0.197(2) 0.4488(13) 0.036 Uiso 1 1 d D . . C1 C -0.05945(18) 0.15190(18) 0.39621(12) 0.0269(4) Uani 1 1 d . . . H1 H -0.0019 0.1031 0.4155 0.032 Uiso 1 1 calc R . . C2 C -0.11949(18) 0.13309(18) 0.33081(12) 0.0297(5) Uani 1 1 d . . . H2 H -0.1117 0.0711 0.2975 0.036 Uiso 1 1 calc R . . C3 C -0.19625(17) 0.22452(17) 0.32216(12) 0.0261(4) Uani 1 1 d . . . C4 C -0.28165(18) 0.25369(18) 0.26941(12) 0.0297(5) Uani 1 1 d . . . H4 H -0.2981 0.2063 0.2273 0.036 Uiso 1 1 calc R . . C5 C -0.34178(18) 0.35200(19) 0.27924(13) 0.0310(5) Uani 1 1 d . . . H5 H -0.4009 0.3711 0.2441 0.037 Uiso 1 1 calc R . . C6 C -0.31694(17) 0.42373(19) 0.34002(12) 0.0290(5) Uani 1 1 d . . . H6 H -0.3578 0.4924 0.3443 0.035 Uiso 1 1 calc R . . C7 C -0.23367(16) 0.39751(17) 0.39483(11) 0.0238(4) Uani 1 1 d . . . C8 C -0.17439(16) 0.29546(17) 0.38572(11) 0.0228(4) Uani 1 1 d . . . C9 C -0.21217(16) 0.47503(17) 0.45585(11) 0.0245(4) Uani 1 1 d . . . H9 H -0.2529 0.5445 0.4548 0.029 Uiso 1 1 calc R . . C10 C -0.07539(17) 0.52887(17) 0.62422(12) 0.0256(4) Uani 1 1 d . . . C11 C 0.5429(2) 0.0428(2) 0.33866(13) 0.0393(6) Uani 1 1 d . . . H11 H 0.5543 0.1145 0.3154 0.047 Uiso 1 1 calc R . . C12 C 0.60269(19) -0.0531(2) 0.32893(13) 0.0362(5) Uani 1 1 d . . . H12 H 0.6617 -0.0611 0.2980 0.043 Uiso 1 1 calc R . . C13 C 0.55935(19) -0.1395(2) 0.37435(14) 0.0353(5) Uani 1 1 d . . . C14 C 0.5865(2) -0.2540(2) 0.3893(2) 0.0570(8) Uani 1 1 d . . . H14 H 0.6442 -0.2903 0.3657 0.068 Uiso 1 1 calc R . . C15 C 0.5273(3) -0.3135(3) 0.4393(3) 0.0791(13) Uani 1 1 d . . . H15 H 0.5448 -0.3914 0.4498 0.095 Uiso 1 1 calc R . . C16 C 0.4429(3) -0.2615(2) 0.4744(2) 0.0674(11) Uani 1 1 d . . . H16 H 0.4045 -0.3050 0.5086 0.081 Uiso 1 1 calc R . . C17 C 0.41277(19) -0.1475(2) 0.46092(15) 0.0382(6) Uani 1 1 d . . . C18 C 0.47250(18) -0.08837(19) 0.41035(13) 0.0307(5) Uani 1 1 d . . . C19 C 0.32384(19) -0.09898(19) 0.49876(14) 0.0355(5) Uani 1 1 d . . . H19 H 0.2891 -0.1449 0.5336 0.043 Uiso 1 1 calc R . . C20 C 0.15805(17) 0.13830(18) 0.52187(12) 0.0258(4) 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 Pd1 0.02199(9) 0.01763(9) 0.02114(9) -0.00008(5) 0.00188(6) 0.00502(5) S1 0.0315(3) 0.0253(3) 0.0232(2) -0.0018(2) -0.0002(2) 0.0066(2) S2 0.0330(3) 0.0271(3) 0.0257(3) 0.0044(2) 0.0064(2) 0.0135(2) N1 0.0233(8) 0.0206(8) 0.0248(9) 0.0000(7) 0.0015(7) 0.0029(6) N2 0.0242(8) 0.0165(8) 0.0249(8) -0.0005(6) 0.0043(7) 0.0014(6) N3 0.0342(9) 0.0171(8) 0.0280(9) -0.0023(7) 0.0050(7) 0.0041(7) N4 0.0507(12) 0.0256(9) 0.0289(10) -0.0053(8) 0.0047(8) 0.0067(8) N5 0.0418(11) 0.0248(9) 0.0370(11) 0.0055(8) 0.0160(8) 0.0064(8) N6 0.0299(9) 0.0276(9) 0.0340(10) 0.0063(8) 0.0112(8) 0.0085(7) N7 0.0311(9) 0.0241(9) 0.0366(10) 0.0083(8) 0.0126(8) 0.0106(7) N8 0.0318(10) 0.0248(9) 0.0344(10) 0.0037(8) 0.0091(8) 0.0095(8) C1 0.0311(11) 0.0195(10) 0.0304(11) -0.0018(8) 0.0045(9) 0.0032(8) C2 0.0375(12) 0.0210(10) 0.0307(11) -0.0048(9) 0.0029(9) -0.0020(9) C3 0.0321(11) 0.0215(10) 0.0249(10) 0.0012(8) 0.0031(8) -0.0066(8) C4 0.0356(11) 0.0282(11) 0.0250(11) 0.0017(9) -0.0001(9) -0.0106(9) C5 0.0298(11) 0.0308(11) 0.0309(12) 0.0070(9) -0.0070(9) -0.0052(9) C6 0.0291(11) 0.0254(10) 0.0319(11) 0.0063(9) -0.0007(9) 0.0002(8) C7 0.0253(10) 0.0203(9) 0.0260(10) 0.0038(8) 0.0029(8) -0.0002(8) C8 0.0240(9) 0.0200(9) 0.0244(10) 0.0019(8) 0.0022(8) -0.0027(7) C9 0.0252(10) 0.0178(9) 0.0306(11) 0.0021(8) 0.0031(8) 0.0040(7) C10 0.0296(10) 0.0213(10) 0.0268(10) -0.0008(8) 0.0069(8) 0.0016(8) C11 0.0504(14) 0.0345(12) 0.0347(13) 0.0072(10) 0.0153(11) 0.0026(11) C12 0.0375(12) 0.0391(13) 0.0336(12) 0.0028(10) 0.0127(10) -0.0006(10) C13 0.0319(11) 0.0326(12) 0.0430(14) 0.0019(10) 0.0135(10) 0.0045(9) C14 0.0489(16) 0.0372(15) 0.090(2) 0.0099(15) 0.0396(16) 0.0165(12) C15 0.073(2) 0.0354(16) 0.137(4) 0.0318(18) 0.065(2) 0.0285(15) C16 0.0627(19) 0.0318(14) 0.116(3) 0.0309(16) 0.059(2) 0.0186(13) C17 0.0356(12) 0.0268(11) 0.0544(16) 0.0102(11) 0.0180(11) 0.0085(9) C18 0.0293(11) 0.0243(11) 0.0393(12) 0.0020(9) 0.0073(9) 0.0045(8) C19 0.0339(12) 0.0258(11) 0.0491(14) 0.0124(10) 0.0172(10) 0.0071(9) C20 0.0270(10) 0.0227(10) 0.0274(11) -0.0012(8) -0.0001(8) 0.0065(8) _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 2.0245(16) . Y Pd1 N1 2.0306(17) . Y Pd1 S1 2.2496(5) . Y Pd1 S2 2.2980(5) . Y S1 C10 1.746(2) . Y S2 C20 1.717(2) . Y N1 C8 1.362(3) . ? N1 C1 1.380(3) . ? N2 C9 1.296(3) . Y N2 N3 1.401(2) . Y N3 C10 1.301(3) . Y N4 C10 1.354(3) . Y N4 H4A 0.8800 . ? N4 H4B 0.8800 . ? N5 C18 1.356(3) . ? N5 C11 1.372(3) . ? N5 H5N 0.8800 . ? N6 C19 1.284(3) . Y N6 N7 1.376(2) . Y N7 C20 1.339(3) . Y N7 H7N 0.876(10) . ? N8 C20 1.315(3) . Y N8 H8A 0.879(10) . ? N8 H8B 0.873(10) . ? C1 C2 1.360(3) . ? C1 H1 0.9500 . ? C2 C3 1.421(3) . ? C2 H2 0.9500 . ? C3 C4 1.400(3) . ? C3 C8 1.424(3) . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C7 1.398(3) . ? C6 H6 0.9500 . ? C7 C8 1.409(3) . ? C7 C9 1.434(3) . ? C9 H9 0.9500 . ? C11 C12 1.354(3) . ? C11 H11 0.9500 . ? C12 C13 1.427(3) . ? C12 H12 0.9500 . ? C13 C14 1.398(4) . ? C13 C18 1.418(3) . ? C14 C15 1.385(4) . ? C14 H14 0.9500 . ? C15 C16 1.390(4) . ? C15 H15 0.9500 . ? C16 C17 1.396(3) . ? C16 H16 0.9500 . ? C17 C18 1.395(3) . ? C17 C19 1.443(3) . ? C19 H19 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 N1 92.43(7) . . Y N2 Pd1 S1 84.58(5) . . Y N1 Pd1 S1 176.77(5) . . Y N2 Pd1 S2 169.53(5) . . Y N1 Pd1 S2 95.25(5) . . Y S1 Pd1 S2 87.86(2) . . Y C10 S1 Pd1 96.45(7) . . ? C20 S2 Pd1 108.61(7) . . Y C8 N1 C1 105.62(17) . . ? C8 N1 Pd1 121.98(13) . . ? C1 N1 Pd1 132.20(14) . . ? C9 N2 N3 113.63(16) . . ? C9 N2 Pd1 126.81(14) . . ? N3 N2 Pd1 119.55(12) . . ? C10 N3 N2 114.53(16) . . ? C10 N4 H4A 120.0 . . ? C10 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C18 N5 C11 108.94(19) . . ? C18 N5 H5N 125.5 . . ? C11 N5 H5N 125.5 . . ? C19 N6 N7 113.53(18) . . ? C20 N7 N6 121.22(18) . . ? C20 N7 H7N 119.4(17) . . ? N6 N7 H7N 119.4(17) . . ? C20 N8 H8A 116.9(18) . . ? C20 N8 H8B 120.3(17) . . ? H8A N8 H8B 123(2) . . ? C2 C1 N1 112.30(19) . . ? C2 C1 H1 123.8 . . ? N1 C1 H1 123.8 . . ? C1 C2 C3 106.38(19) . . ? C1 C2 H2 126.8 . . ? C3 C2 H2 126.8 . . ? C4 C3 C2 135.1(2) . . ? C4 C3 C8 119.4(2) . . ? C2 C3 C8 105.43(18) . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.9(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 121.9(2) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 C8 117.03(19) . . ? C6 C7 C9 119.14(18) . . ? C8 C7 C9 123.82(18) . . ? N1 C8 C7 128.51(19) . . ? N1 C8 C3 110.25(18) . . ? C7 C8 C3 121.24(19) . . ? N2 C9 C7 125.61(18) . . ? N2 C9 H9 117.2 . . ? C7 C9 H9 117.2 . . ? N3 C10 N4 118.39(19) . . ? N3 C10 S1 124.67(16) . . ? N4 C10 S1 116.93(16) . . ? C12 C11 N5 110.4(2) . . ? C12 C11 H11 124.8 . . ? N5 C11 H11 124.8 . . ? C11 C12 C13 106.3(2) . . ? C11 C12 H12 126.8 . . ? C13 C12 H12 126.8 . . ? C14 C13 C18 119.2(2) . . ? C14 C13 C12 133.9(2) . . ? C18 C13 C12 106.8(2) . . ? C15 C14 C13 118.4(2) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C14 C15 C16 121.4(2) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C17 122.0(2) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C18 C17 C16 116.2(2) . . ? C18 C17 C19 124.5(2) . . ? C16 C17 C19 119.3(2) . . ? N5 C18 C17 129.9(2) . . ? N5 C18 C13 107.43(19) . . ? C17 C18 C13 122.6(2) . . ? N6 C19 C17 122.3(2) . . ? N6 C19 H19 118.9 . . ? C17 C19 H19 118.9 . . ? N8 C20 N7 120.25(19) . . ? N8 C20 S2 124.74(16) . . ? N7 C20 S2 114.99(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5N N6 0.88 2.40 2.900(3) 116.0 . N8 H8A N3 0.879(10) 2.109(15) 2.928(2) 155(2) 3_566 N4 H4B Cg1 0.88 2.78 3.619(2) 160 4_566 C19 H19 Cg2 0.95 2.79 3.689(3) 158 3_556 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.835 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.076 loop_ _shelx_res_file ; TITL [Pd(L)(LH2)] CELL 0.71073 12.2138 11.6637 18.0652 90.000 94.385 90.000 ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N S Pd UNIT 80 72 32 8 4 OMIT -2 55 L.S. 16 HTAB N5 N6 HTAB N8 N3_$1 EQIV $1 -X, -Y+1, -Z+1 mpla c1 > c10 n1 > n4 s1 mpla c11 > c20 n5 > n8 s2 mpla 4 n1 n2 s1 s2 pd1 ACTA BOND $h SIZE 0.21 0.28 0.32 DFIX 0.88 0.01 N7 H7N N8 H8A N8 H8B TEMP -173 WGHT 0.036400 0.523600 FVAR 1.00976 PD1 5 -0.046164 0.318521 0.532344 11.00000 0.02199 0.01763 = 0.02114 -0.00008 0.00188 0.00502 S1 4 0.001481 0.404211 0.641645 11.00000 0.03150 0.02532 = 0.02317 -0.00175 -0.00016 0.00664 S2 4 0.050545 0.160377 0.576143 11.00000 0.03300 0.02710 = 0.02574 0.00444 0.00645 0.01350 N1 3 -0.091609 0.249993 0.431311 11.00000 0.02334 0.02057 = 0.02478 0.00000 0.00152 0.00290 N2 3 -0.141982 0.458442 0.512362 11.00000 0.02416 0.01645 = 0.02492 -0.00051 0.00433 0.00145 N3 3 -0.137195 0.548675 0.563705 11.00000 0.03420 0.01710 = 0.02800 -0.00227 0.00501 0.00405 N4 3 -0.071259 0.608817 0.678693 11.00000 0.05068 0.02564 = 0.02889 -0.00533 0.00466 0.00673 AFIX 93 H4A 2 -0.109822 0.672317 0.672667 11.00000 -1.20000 H4B 2 -0.030014 0.597287 0.720124 11.00000 -1.20000 AFIX 0 N5 3 0.463655 0.021894 0.386786 11.00000 0.04178 0.02476 = 0.03699 0.00554 0.01604 0.00640 AFIX 43 H5N 2 0.414971 0.071890 0.400202 11.00000 -1.20000 AFIX 0 N6 3 0.289971 0.004103 0.487029 11.00000 0.02991 0.02758 = 0.03402 0.00631 0.01115 0.00846 N7 3 0.204307 0.034300 0.528266 11.00000 0.03109 0.02409 = 0.03660 0.00830 0.01258 0.01056 H7N 2 0.178519 -0.015982 0.558511 11.00000 -1.20000 N8 3 0.193491 0.213702 0.475159 11.00000 0.03184 0.02481 = 0.03438 0.00365 0.00914 0.00945 H8A 2 0.161580 0.281254 0.473670 11.00000 -1.20000 H8B 2 0.248295 0.196987 0.448777 11.00000 -1.20000 C1 1 -0.059451 0.151897 0.396209 11.00000 0.03105 0.01952 = 0.03042 -0.00176 0.00449 0.00325 AFIX 43 H1 2 -0.001922 0.103057 0.415526 11.00000 -1.20000 AFIX 0 C2 1 -0.119491 0.133092 0.330806 11.00000 0.03749 0.02095 = 0.03068 -0.00482 0.00286 -0.00200 AFIX 43 H2 2 -0.111656 0.071109 0.297506 11.00000 -1.20000 AFIX 0 C3 1 -0.196250 0.224517 0.322157 11.00000 0.03210 0.02149 = 0.02492 0.00125 0.00307 -0.00661 C4 1 -0.281651 0.253691 0.269409 11.00000 0.03559 0.02816 = 0.02505 0.00166 -0.00011 -0.01055 AFIX 43 H4 2 -0.298069 0.206290 0.227252 11.00000 -1.20000 AFIX 0 C5 1 -0.341775 0.352002 0.279244 11.00000 0.02978 0.03078 = 0.03086 0.00703 -0.00700 -0.00516 AFIX 43 H5 2 -0.400874 0.371077 0.244149 11.00000 -1.20000 AFIX 0 C6 1 -0.316936 0.423726 0.340017 11.00000 0.02913 0.02543 = 0.03194 0.00632 -0.00068 0.00019 AFIX 43 H6 2 -0.357805 0.492396 0.344279 11.00000 -1.20000 AFIX 0 C7 1 -0.233669 0.397508 0.394826 11.00000 0.02526 0.02027 = 0.02604 0.00380 0.00289 -0.00022 C8 1 -0.174393 0.295463 0.385719 11.00000 0.02397 0.02005 = 0.02442 0.00188 0.00221 -0.00275 C9 1 -0.212172 0.475034 0.455852 11.00000 0.02518 0.01776 = 0.03057 0.00213 0.00310 0.00401 AFIX 43 H9 2 -0.252867 0.544504 0.454764 11.00000 -1.20000 AFIX 0 C10 1 -0.075386 0.528867 0.624224 11.00000 0.02956 0.02128 = 0.02682 -0.00076 0.00689 0.00160 C11 1 0.542905 0.042822 0.338656 11.00000 0.05043 0.03451 = 0.03472 0.00723 0.01535 0.00255 AFIX 43 H11 2 0.554256 0.114460 0.315420 11.00000 -1.20000 AFIX 0 C12 1 0.602694 -0.053054 0.328931 11.00000 0.03752 0.03910 = 0.03360 0.00279 0.01271 -0.00060 AFIX 43 H12 2 0.661745 -0.061145 0.298020 11.00000 -1.20000 AFIX 0 C13 1 0.559350 -0.139517 0.374352 11.00000 0.03190 0.03257 = 0.04299 0.00189 0.01348 0.00449 C14 1 0.586497 -0.254038 0.389276 11.00000 0.04886 0.03724 = 0.09023 0.00986 0.03957 0.01647 AFIX 43 H14 2 0.644192 -0.290265 0.365694 11.00000 -1.20000 AFIX 0 C15 1 0.527314 -0.313467 0.439252 11.00000 0.07321 0.03542 = 0.13733 0.03177 0.06531 0.02848 AFIX 43 H15 2 0.544792 -0.391437 0.449768 11.00000 -1.20000 AFIX 0 C16 1 0.442870 -0.261526 0.474376 11.00000 0.06265 0.03184 = 0.11591 0.03090 0.05929 0.01858 AFIX 43 H16 2 0.404488 -0.304952 0.508584 11.00000 -1.20000 AFIX 0 C17 1 0.412773 -0.147548 0.460917 11.00000 0.03560 0.02680 = 0.05440 0.01015 0.01798 0.00848 C18 1 0.472499 -0.088368 0.410349 11.00000 0.02928 0.02429 = 0.03933 0.00201 0.00730 0.00454 C19 1 0.323837 -0.098975 0.498756 11.00000 0.03392 0.02578 = 0.04908 0.01243 0.01717 0.00712 AFIX 43 H19 2 0.289128 -0.144875 0.533564 11.00000 -1.20000 AFIX 0 C20 1 0.158050 0.138302 0.521871 11.00000 0.02700 0.02275 = 0.02736 -0.00116 -0.00012 0.00647 HKLF 4 REM sad in P2(1)/n REM R1 = 0.0265 for 5136 Fo > 4sig(Fo) and 0.0312 for all 5866 data REM 289 parameters refined using 3 restraints END WGHT 0.0364 0.5235 REM Highest difference peak 0.835, deepest hole -0.377, 1-sigma level 0.076 Q1 1 0.2042 0.2849 0.4581 11.00000 0.05 0.84 Q2 1 0.1391 0.2796 0.4841 11.00000 0.05 0.60 Q3 1 -0.0024 0.2977 0.5027 11.00000 0.05 0.52 Q4 1 0.0150 0.3751 0.6008 11.00000 0.05 0.50 ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 -0.023 0.250 327 62 ' ' 2 0.750 -0.028 0.750 327 62 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 939911' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[Pd(L)(PPh3)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H23 N4 P Pd S, C3 H7 N O' _chemical_formula_sum 'C31 H30 N5 O P Pd S' _chemical_formula_weight 658.03 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' Pd Pd -0.9988 1.0072 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6267(5) _cell_length_b 10.0243(5) _cell_length_c 15.6913(8) _cell_angle_alpha 80.642(3) _cell_angle_beta 87.833(3) _cell_angle_gamma 73.852(3) _cell_volume 1435.08(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4510 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 30.85 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7875 _exptl_absorpt_correction_T_max 0.9162 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8518 _diffrn_reflns_av_R_equivalents 0.0111 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5094 _reflns_number_gt 4821 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0261P)^2^+1.2453P] 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 5094 _refine_ls_number_parameters 399 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0538 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _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 0.975089(15) 0.249931(14) 0.240970(9) 0.01444(5) Uani 1 1 d . . . S1 S 0.79729(5) 0.27261(5) 0.14556(3) 0.02362(11) Uani 1 1 d . . . P1 P 0.82153(5) 0.40599(5) 0.31447(3) 0.01454(10) Uani 1 1 d . . . N1 N 1.14613(17) 0.21782(16) 0.32252(10) 0.0164(3) Uani 1 1 d . . . N2 N 1.09976(18) 0.11908(16) 0.16114(10) 0.0196(3) Uani 1 1 d . . . N3 N 1.0362(2) 0.09238(19) 0.08938(11) 0.0279(4) Uani 1 1 d . . . N4 N 0.8304(2) 0.1453(2) 0.00824(14) 0.0402(5) Uani 1 1 d D . . H4A H 0.7381(19) 0.162(3) 0.0090(19) 0.048 Uiso 1 1 d D . . H4B H 0.878(3) 0.077(2) -0.0194(17) 0.048 Uiso 1 1 d D . . C1 C 1.1583(2) 0.26359(19) 0.39983(12) 0.0175(4) Uani 1 1 d . . . H1 H 1.0809 0.3248 0.4258 0.021 Uiso 1 1 calc R . . C2 C 1.2945(2) 0.2108(2) 0.43458(12) 0.0193(4) Uani 1 1 d . . . H2 H 1.3271 0.2271 0.4873 0.023 Uiso 1 1 calc R . . C3 C 1.3774(2) 0.12643(19) 0.37581(12) 0.0183(4) Uani 1 1 d . . . C4 C 1.5225(2) 0.0485(2) 0.37275(14) 0.0225(4) Uani 1 1 d . . . H4 H 1.5868 0.0397 0.4191 0.027 Uiso 1 1 calc R . . C5 C 1.5712(2) -0.0156(2) 0.30117(14) 0.0249(4) Uani 1 1 d . . . H5 H 1.6700 -0.0665 0.2980 0.030 Uiso 1 1 calc R . . C6 C 1.4775(2) -0.0067(2) 0.23403(13) 0.0229(4) Uani 1 1 d . . . H6 H 1.5143 -0.0504 0.1854 0.028 Uiso 1 1 calc R . . C7 C 1.3295(2) 0.06553(19) 0.23597(13) 0.0191(4) Uani 1 1 d . . . C8 C 1.2811(2) 0.13434(19) 0.30745(12) 0.0165(4) Uani 1 1 d . . . C9 C 1.2381(2) 0.06141(19) 0.16713(12) 0.0205(4) Uani 1 1 d . . . H9 H 1.2826 0.0122 0.1220 0.025 Uiso 1 1 calc R . . C10 C 0.8996(2) 0.1594(2) 0.07810(13) 0.0277(5) Uani 1 1 d . . . C11 C 0.88806(19) 0.56022(19) 0.31124(13) 0.0179(4) Uani 1 1 d . . . C12 C 0.9225(2) 0.6213(2) 0.22969(14) 0.0255(4) Uani 1 1 d . . . H12 H 0.9159 0.5787 0.1807 0.031 Uiso 1 1 calc R . . C13 C 0.9662(2) 0.7440(2) 0.21943(15) 0.0283(5) Uani 1 1 d . . . H13 H 0.9862 0.7867 0.1635 0.034 Uiso 1 1 calc R . . C14 C 0.9805(2) 0.8036(2) 0.29096(15) 0.0267(5) Uani 1 1 d . . . H14 H 1.0106 0.8873 0.2843 0.032 Uiso 1 1 calc R . . C15 C 0.9509(2) 0.7415(2) 0.37196(15) 0.0279(5) Uani 1 1 d . . . H15 H 0.9632 0.7815 0.4211 0.033 Uiso 1 1 calc R . . C16 C 0.9035(2) 0.6210(2) 0.38259(13) 0.0234(4) Uani 1 1 d . . . H16 H 0.8817 0.5801 0.4386 0.028 Uiso 1 1 calc R . . C17 C 0.78904(19) 0.33315(19) 0.42489(12) 0.0161(4) Uani 1 1 d . . . C18 C 0.7015(2) 0.4168(2) 0.48009(12) 0.0202(4) Uani 1 1 d . . . H18 H 0.6681 0.5157 0.4628 0.024 Uiso 1 1 calc R . . C19 C 0.6632(2) 0.3561(2) 0.56007(13) 0.0233(4) Uani 1 1 d . . . H19 H 0.6061 0.4136 0.5981 0.028 Uiso 1 1 calc R . . C20 C 0.7084(2) 0.2111(2) 0.58455(13) 0.0223(4) Uani 1 1 d . . . H20 H 0.6803 0.1695 0.6388 0.027 Uiso 1 1 calc R . . C21 C 0.7943(2) 0.1269(2) 0.53003(13) 0.0199(4) Uani 1 1 d . . . H21 H 0.8248 0.0278 0.5470 0.024 Uiso 1 1 calc R . . C22 C 0.8358(2) 0.18737(19) 0.45047(12) 0.0171(4) Uani 1 1 d . . . H22 H 0.8960 0.1297 0.4136 0.020 Uiso 1 1 calc R . . C23 C 0.6360(2) 0.47718(19) 0.27358(12) 0.0162(4) Uani 1 1 d . . . C24 C 0.5493(2) 0.3848(2) 0.28052(13) 0.0239(4) Uani 1 1 d . . . H24 H 0.5880 0.2891 0.3056 0.029 Uiso 1 1 calc R . . C25 C 0.4079(2) 0.4314(2) 0.25120(14) 0.0269(5) Uani 1 1 d . . . H25 H 0.3495 0.3681 0.2568 0.032 Uiso 1 1 calc R . . C26 C 0.3511(2) 0.5699(2) 0.21368(14) 0.0252(4) Uani 1 1 d . . . H26 H 0.2544 0.6015 0.1925 0.030 Uiso 1 1 calc R . . C27 C 0.4355(2) 0.6621(2) 0.20705(14) 0.0260(4) Uani 1 1 d . . . H27 H 0.3962 0.7575 0.1817 0.031 Uiso 1 1 calc R . . C28 C 0.5775(2) 0.6166(2) 0.23706(12) 0.0196(4) Uani 1 1 d . . . H28 H 0.6346 0.6810 0.2326 0.024 Uiso 1 1 calc R . . O1 O 0.5281(3) 0.1513(3) -0.0314(2) 0.0331(10) Uani 0.544(4) 1 d PG A 1 N5 N 0.3434(3) 0.3279(3) 0.00304(16) 0.0380(13) Uani 0.544(4) 1 d PG A 1 C29 C 0.4000(3) 0.2034(3) -0.01976(17) 0.0330(11) Uani 0.544(4) 1 d PG A 1 H29 H 0.3368 0.1510 -0.0276 0.040 Uiso 0.544(4) 1 d PG A 1 C30 C 0.1890(3) 0.3851(4) 0.0128(3) 0.048(2) Uani 0.544(4) 1 d PG A 1 H30A H 0.1391 0.3172 0.0008 0.072 Uiso 0.544(4) 1 calc PR A 1 H30B H 0.1551 0.4729 -0.0278 0.072 Uiso 0.544(4) 1 calc PR A 1 H30C H 0.1684 0.4039 0.0720 0.072 Uiso 0.544(4) 1 calc PR A 1 C31 C 0.4360(4) 0.4152(3) 0.0138(3) 0.0437(13) Uani 0.544(4) 1 d PG A 1 H31A H 0.4880 0.3806 0.0690 0.066 Uiso 0.544(4) 1 calc PR A 1 H31B H 0.3771 0.5124 0.0131 0.066 Uiso 0.544(4) 1 calc PR A 1 H31C H 0.5057 0.4118 -0.0335 0.066 Uiso 0.544(4) 1 calc PR A 1 O2 O 0.5467(3) 0.1606(5) 0.0052(3) 0.0408(13) Uani 0.456(4) 1 d PG A 2 N6 N 0.3122(3) 0.2822(3) 0.01075(19) 0.0325(15) Uani 0.456(4) 1 d PG A 2 C32 C 0.4504(3) 0.2528(4) 0.0304(2) 0.0416(15) Uani 0.456(4) 1 d PG A 2 H32 H 0.4767 0.3070 0.0664 0.050 Uiso 0.456(4) 1 d PG A 2 C33 C 0.2031(5) 0.3906(5) 0.0456(4) 0.045(2) Uani 0.456(4) 1 d PG A 2 H33A H 0.2481 0.4288 0.0875 0.068 Uiso 0.456(4) 1 calc PR A 2 H33B H 0.1286 0.3502 0.0744 0.068 Uiso 0.456(4) 1 calc PR A 2 H33C H 0.1589 0.4660 -0.0013 0.068 Uiso 0.456(4) 1 calc PR A 2 C34 C 0.2651(4) 0.1989(5) -0.0429(3) 0.0429(15) Uani 0.456(4) 1 d PG A 2 H34A H 0.2658 0.2418 -0.1036 0.064 Uiso 0.456(4) 1 calc PR A 2 H34B H 0.1668 0.1949 -0.0268 0.064 Uiso 0.456(4) 1 calc PR A 2 H34C H 0.3306 0.1035 -0.0348 0.064 Uiso 0.456(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01579(8) 0.01366(8) 0.01358(8) -0.00398(5) -0.00136(5) -0.00236(5) S1 0.0222(3) 0.0261(3) 0.0218(2) -0.0101(2) -0.0061(2) -0.0011(2) P1 0.0152(2) 0.0127(2) 0.0154(2) -0.00282(18) -0.00037(18) -0.00293(18) N1 0.0171(8) 0.0154(8) 0.0167(8) -0.0039(6) -0.0006(6) -0.0035(6) N2 0.0250(9) 0.0169(8) 0.0167(8) -0.0064(6) -0.0019(7) -0.0029(7) N3 0.0327(10) 0.0279(9) 0.0219(9) -0.0140(7) -0.0074(7) 0.0000(8) N4 0.0385(12) 0.0433(12) 0.0370(12) -0.0261(10) -0.0156(10) 0.0052(10) C1 0.0201(10) 0.0154(9) 0.0170(9) -0.0046(7) 0.0003(7) -0.0038(7) C2 0.0204(10) 0.0195(10) 0.0188(9) -0.0038(8) -0.0028(8) -0.0063(8) C3 0.0190(10) 0.0154(9) 0.0216(10) -0.0011(7) -0.0009(8) -0.0070(7) C4 0.0194(10) 0.0176(10) 0.0303(11) -0.0005(8) -0.0040(8) -0.0060(8) C5 0.0171(10) 0.0187(10) 0.0368(12) -0.0033(9) 0.0030(9) -0.0026(8) C6 0.0235(11) 0.0177(10) 0.0266(11) -0.0046(8) 0.0063(8) -0.0042(8) C7 0.0203(10) 0.0146(9) 0.0211(10) -0.0012(7) 0.0022(8) -0.0038(7) C8 0.0167(9) 0.0129(9) 0.0198(9) -0.0008(7) 0.0007(7) -0.0049(7) C9 0.0274(11) 0.0141(9) 0.0183(9) -0.0045(7) 0.0038(8) -0.0022(8) C10 0.0355(12) 0.0246(11) 0.0219(10) -0.0103(9) -0.0063(9) -0.0021(9) C11 0.0116(9) 0.0151(9) 0.0257(10) -0.0031(8) -0.0003(7) -0.0016(7) C12 0.0269(11) 0.0241(10) 0.0281(11) -0.0095(9) 0.0088(9) -0.0094(9) C13 0.0249(11) 0.0255(11) 0.0346(12) -0.0030(9) 0.0102(9) -0.0097(9) C14 0.0167(10) 0.0196(10) 0.0452(13) -0.0052(9) 0.0007(9) -0.0071(8) C15 0.0287(12) 0.0234(10) 0.0348(12) -0.0068(9) -0.0088(9) -0.0103(9) C16 0.0245(11) 0.0211(10) 0.0246(10) -0.0014(8) -0.0055(8) -0.0068(8) C17 0.0145(9) 0.0174(9) 0.0167(9) -0.0027(7) -0.0015(7) -0.0047(7) C18 0.0212(10) 0.0164(9) 0.0206(10) -0.0026(8) -0.0013(8) -0.0012(8) C19 0.0206(10) 0.0275(11) 0.0203(10) -0.0072(8) 0.0018(8) -0.0025(8) C20 0.0204(10) 0.0286(11) 0.0181(10) -0.0015(8) 0.0002(8) -0.0082(8) C21 0.0193(10) 0.0180(9) 0.0223(10) -0.0001(8) -0.0026(8) -0.0063(8) C22 0.0164(9) 0.0163(9) 0.0191(9) -0.0045(7) -0.0010(7) -0.0044(7) C23 0.0156(9) 0.0165(9) 0.0151(9) -0.0032(7) 0.0012(7) -0.0021(7) C24 0.0232(11) 0.0191(10) 0.0286(11) 0.0020(8) -0.0042(8) -0.0070(8) C25 0.0236(11) 0.0289(11) 0.0304(11) -0.0019(9) -0.0014(9) -0.0121(9) C26 0.0157(10) 0.0281(11) 0.0305(11) -0.0077(9) -0.0024(8) -0.0019(8) C27 0.0243(11) 0.0186(10) 0.0314(11) -0.0018(9) -0.0056(9) -0.0003(8) C28 0.0193(10) 0.0173(9) 0.0219(10) -0.0033(8) 0.0009(8) -0.0045(8) O1 0.031(2) 0.0360(18) 0.025(2) -0.0020(16) -0.0010(15) 0.0014(15) N5 0.034(3) 0.041(3) 0.035(2) -0.0111(19) -0.0118(19) 0.000(2) C29 0.035(3) 0.038(2) 0.021(2) 0.0019(18) -0.0003(18) -0.007(2) C30 0.040(3) 0.059(4) 0.019(4) 0.020(2) 0.014(2) 0.012(3) C31 0.040(3) 0.043(3) 0.045(3) -0.018(2) -0.009(2) 0.001(2) O2 0.026(2) 0.051(3) 0.040(3) 0.004(2) -0.010(2) -0.008(2) N6 0.023(3) 0.040(3) 0.037(3) -0.013(2) -0.006(2) -0.008(2) C32 0.040(3) 0.045(3) 0.042(3) 0.013(3) -0.017(3) -0.024(3) C33 0.044(4) 0.042(4) 0.036(5) 0.022(3) 0.000(3) -0.006(3) C34 0.034(3) 0.070(4) 0.029(3) -0.001(3) -0.003(2) -0.023(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 2.0452(15) . Y Pd1 N2 2.0676(16) . Y Pd1 S1 2.2560(5) . Y Pd1 P1 2.2658(5) . Y S1 C10 1.752(2) . Y P1 C17 1.8188(19) . ? P1 C11 1.8236(19) . ? P1 C23 1.8278(19) . ? N1 C8 1.372(2) . ? N1 C1 1.385(2) . ? N2 C9 1.296(3) . Y N2 N3 1.398(2) . Y N3 C10 1.303(3) . Y N4 C10 1.350(3) . Y N4 H4A 0.857(17) . ? N4 H4B 0.879(17) . ? C1 C2 1.367(3) . ? C1 H1 0.9500 . ? C2 C3 1.423(3) . ? C2 H2 0.9500 . ? C3 C4 1.402(3) . ? C3 C8 1.422(3) . ? C4 C5 1.386(3) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 C7 1.409(3) . ? C6 H6 0.9500 . ? C7 C8 1.409(3) . ? C7 C9 1.432(3) . ? C9 H9 0.9500 . ? C11 C16 1.390(3) . ? C11 C12 1.396(3) . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 C14 1.382(3) . ? C13 H13 0.9500 . ? C14 C15 1.378(3) . ? C14 H14 0.9500 . ? C15 C16 1.390(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.397(3) . ? C17 C22 1.399(3) . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 C20 1.389(3) . ? C19 H19 0.9500 . ? C20 C21 1.386(3) . ? C20 H20 0.9500 . ? C21 C22 1.392(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.388(3) . ? C23 C24 1.399(3) . ? C24 C25 1.381(3) . ? C24 H24 0.9500 . ? C25 C26 1.382(3) . ? C25 H25 0.9500 . ? C26 C27 1.381(3) . ? C26 H26 0.9500 . ? C27 C28 1.389(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? O1 C29 1.2179 . ? N5 C29 1.3175 . ? N5 C31 1.4416 . ? N5 C30 1.4487 . ? C29 H29 0.9300 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C31 H32 1.2276 . ? O2 C32 1.2179 . ? N6 C32 1.3175 . ? N6 C34 1.4416 . ? N6 C33 1.4488 . ? C32 H32 0.9300 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H29 0.7456 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 91.89(6) . . Y N1 Pd1 S1 175.59(4) . . Y N2 Pd1 S1 83.73(5) . . Y N1 Pd1 P1 94.30(4) . . Y N2 Pd1 P1 173.16(5) . . Y S1 Pd1 P1 90.092(18) . . Y C10 S1 Pd1 97.17(7) . . ? C17 P1 C11 111.16(9) . . ? C17 P1 C23 100.49(8) . . ? C11 P1 C23 104.39(8) . . ? C17 P1 Pd1 113.99(6) . . ? C11 P1 Pd1 109.28(6) . . ? C23 P1 Pd1 116.92(6) . . ? C8 N1 C1 105.38(15) . . ? C8 N1 Pd1 122.17(12) . . ? C1 N1 Pd1 132.43(13) . . ? C9 N2 N3 113.55(16) . . ? C9 N2 Pd1 126.63(13) . . ? N3 N2 Pd1 119.71(12) . . ? C10 N3 N2 114.40(16) . . ? C10 N4 H4A 119(2) . . ? C10 N4 H4B 114.8(19) . . ? H4A N4 H4B 117(3) . . ? C2 C1 N1 112.39(17) . . ? C2 C1 H1 123.8 . . ? N1 C1 H1 123.8 . . ? C1 C2 C3 106.13(17) . . ? C1 C2 H2 126.9 . . ? C3 C2 H2 126.9 . . ? C4 C3 C8 119.86(18) . . ? C4 C3 C2 134.25(18) . . ? C8 C3 C2 105.87(16) . . ? C5 C4 C3 119.14(19) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 120.96(19) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 121.87(19) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C8 C7 C6 117.12(18) . . ? C8 C7 C9 124.42(18) . . ? C6 C7 C9 118.44(17) . . ? N1 C8 C7 128.78(17) . . ? N1 C8 C3 110.23(16) . . ? C7 C8 C3 120.97(17) . . ? N2 C9 C7 125.61(17) . . ? N2 C9 H9 117.2 . . ? C7 C9 H9 117.2 . . ? N3 C10 N4 118.72(19) . . ? N3 C10 S1 124.94(15) . . ? N4 C10 S1 116.31(17) . . ? C16 C11 C12 118.90(18) . . ? C16 C11 P1 125.06(15) . . ? C12 C11 P1 116.02(15) . . ? C13 C12 C11 120.6(2) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 119.8(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 119.88(19) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.7(2) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C11 C16 C15 120.01(19) . . ? C11 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C22 119.39(17) . . ? C18 C17 P1 121.26(14) . . ? C22 C17 P1 118.72(14) . . ? C19 C18 C17 120.31(18) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 119.99(18) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 120.20(18) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.14(18) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C17 119.94(17) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? C28 C23 C24 118.99(18) . . ? C28 C23 P1 123.61(15) . . ? C24 C23 P1 117.40(14) . . ? C25 C24 C23 120.53(19) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.18(19) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 119.70(19) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 120.61(19) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C23 C28 C27 119.97(18) . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C29 N5 C31 119.6 . . ? C29 N5 C30 122.2 . . ? C31 N5 C30 118.1 . . ? O1 C29 N5 125.4 . . ? C32 N6 C34 119.6 . . ? C32 N6 C33 122.2 . . ? C34 N6 C33 118.1 . . ? C32 N6 H29 91.6 . . ? C33 N6 H29 144.0 . . ? O2 C32 N6 125.4 . . ? O2 C32 H32 117.3 . . ? N6 C32 H32 117.3 . . ? N6 C33 H33A 109.5 . . ? N6 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N6 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N6 C34 H29 78.9 . . ? N6 C34 H34A 109.5 . . ? N6 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N6 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4B N3 0.879(17) 2.129(18) 3.001(3) 172(3) 2_755 N4 H4A O1 0.857(17) 2.18(2) 2.982(4) 156(3) . N4 H4A O2 0.857(17) 1.851(18) 2.695(4) 168(3) . C15 H15 Cg1 0.95 2.92 3.497(2) 120 2_766 C19 H19 Cg2 0.95 2.73 3.609(2) 154 2_666 C20 H20 Cg3 0.95 2.77 3.505(2) 135 2_756 C21 H21 Cg4 0.95 2.64 3.457(2) 144 2_756 C25 H25 Cg4 0.95 2.63 3.439(2) 144 1_455 C25 H25 Cg3 0.95 2.96 3.648(2) 131 1_455 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.333 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.057 loop_ _shelx_res_file ; TITL sad in [Pd(L)(PPh3)] CELL 0.71073 9.6267 10.0243 15.6913 80.642 87.833 73.852 ZERR 2 0.0005 0.0005 0.0008 0.001 0.001 0.001 LATT 1 SFAC C H N O P Pd S UNIT 62 60 10 2 2 2 2 OMIT -2 50.5 L.S. 8 OMIT 1 4 10 size 0.31 0.22 0.11 temp -173 ACTA BOND $H DFIX 0.88 N4 H4A N4 H4B WGHT 0.026100 1.245300 FVAR 0.36570 0.54408 PD1 6 0.975089 0.249931 0.240970 11.00000 0.01579 0.01366 = 0.01358 -0.00398 -0.00136 -0.00236 S1 7 0.797291 0.272605 0.145557 11.00000 0.02222 0.02613 = 0.02183 -0.01012 -0.00614 -0.00114 P1 5 0.821535 0.405995 0.314465 11.00000 0.01521 0.01271 = 0.01540 -0.00282 -0.00037 -0.00293 N1 3 1.146130 0.217817 0.322518 11.00000 0.01712 0.01541 = 0.01675 -0.00391 -0.00064 -0.00353 N2 3 1.099760 0.119077 0.161142 11.00000 0.02500 0.01690 = 0.01674 -0.00643 -0.00187 -0.00289 N3 3 1.036160 0.092384 0.089384 11.00000 0.03273 0.02794 = 0.02195 -0.01396 -0.00737 0.00003 N4 3 0.830439 0.145290 0.008241 11.00000 0.03845 0.04333 = 0.03699 -0.02612 -0.01556 0.00516 H4A 2 0.738147 0.162270 0.008976 11.00000 -1.20000 H4B 2 0.878153 0.077116 -0.019358 11.00000 -1.20000 C1 1 1.158337 0.263588 0.399829 11.00000 0.02008 0.01539 = 0.01700 -0.00463 0.00028 -0.00382 AFIX 43 H1 2 1.080851 0.324788 0.425792 11.00000 -1.20000 AFIX 0 C2 1 1.294480 0.210772 0.434584 11.00000 0.02037 0.01954 = 0.01885 -0.00376 -0.00284 -0.00629 AFIX 43 H2 2 1.327118 0.227082 0.487323 11.00000 -1.20000 AFIX 0 C3 1 1.377417 0.126435 0.375805 11.00000 0.01896 0.01536 = 0.02156 -0.00113 -0.00092 -0.00701 C4 1 1.522544 0.048472 0.372746 11.00000 0.01937 0.01758 = 0.03032 -0.00050 -0.00399 -0.00605 AFIX 43 H4 2 1.586751 0.039686 0.419134 11.00000 -1.20000 AFIX 0 C5 1 1.571168 -0.015638 0.301165 11.00000 0.01714 0.01871 = 0.03683 -0.00331 0.00295 -0.00258 AFIX 43 H5 2 1.670018 -0.066460 0.298016 11.00000 -1.20000 AFIX 0 C6 1 1.477534 -0.006662 0.234025 11.00000 0.02350 0.01772 = 0.02657 -0.00461 0.00633 -0.00425 AFIX 43 H6 2 1.514280 -0.050443 0.185382 11.00000 -1.20000 AFIX 0 C7 1 1.329544 0.065535 0.235966 11.00000 0.02028 0.01463 = 0.02106 -0.00120 0.00222 -0.00383 C8 1 1.281136 0.134343 0.307448 11.00000 0.01671 0.01291 = 0.01983 -0.00078 0.00065 -0.00488 C9 1 1.238066 0.061407 0.167135 11.00000 0.02738 0.01408 = 0.01835 -0.00449 0.00383 -0.00223 AFIX 43 H9 2 1.282591 0.012158 0.121982 11.00000 -1.20000 AFIX 0 C10 1 0.899624 0.159355 0.078099 11.00000 0.03555 0.02461 = 0.02187 -0.01029 -0.00633 -0.00208 C11 1 0.888057 0.560222 0.311240 11.00000 0.01163 0.01508 = 0.02568 -0.00314 -0.00025 -0.00161 C12 1 0.922463 0.621312 0.229688 11.00000 0.02691 0.02414 = 0.02814 -0.00948 0.00885 -0.00939 AFIX 43 H12 2 0.915935 0.578680 0.180714 11.00000 -1.20000 AFIX 0 C13 1 0.966223 0.744027 0.219429 11.00000 0.02492 0.02553 = 0.03459 -0.00303 0.01021 -0.00971 AFIX 43 H13 2 0.986249 0.786717 0.163458 11.00000 -1.20000 AFIX 0 C14 1 0.980464 0.803634 0.290962 11.00000 0.01669 0.01964 = 0.04517 -0.00518 0.00073 -0.00712 AFIX 43 H14 2 1.010552 0.887298 0.284276 11.00000 -1.20000 AFIX 0 C15 1 0.950949 0.741499 0.371955 11.00000 0.02875 0.02335 = 0.03481 -0.00675 -0.00878 -0.01029 AFIX 43 H15 2 0.963151 0.781481 0.421095 11.00000 -1.20000 AFIX 0 C16 1 0.903517 0.620964 0.382588 11.00000 0.02447 0.02114 = 0.02465 -0.00145 -0.00553 -0.00677 AFIX 43 H16 2 0.881662 0.580098 0.438643 11.00000 -1.20000 AFIX 0 C17 1 0.789041 0.333147 0.424895 11.00000 0.01450 0.01744 = 0.01670 -0.00270 -0.00152 -0.00475 C18 1 0.701511 0.416768 0.480088 11.00000 0.02121 0.01644 = 0.02064 -0.00261 -0.00134 -0.00121 AFIX 43 H18 2 0.668059 0.515703 0.462754 11.00000 -1.20000 AFIX 0 C19 1 0.663208 0.356053 0.560072 11.00000 0.02064 0.02749 = 0.02026 -0.00720 0.00178 -0.00252 AFIX 43 H19 2 0.606066 0.413628 0.598107 11.00000 -1.20000 AFIX 0 C20 1 0.708392 0.211086 0.584554 11.00000 0.02043 0.02860 = 0.01808 -0.00152 0.00024 -0.00820 AFIX 43 H20 2 0.680342 0.169462 0.638849 11.00000 -1.20000 AFIX 0 C21 1 0.794274 0.126946 0.530033 11.00000 0.01933 0.01802 = 0.02232 -0.00012 -0.00265 -0.00632 AFIX 43 H21 2 0.824840 0.027798 0.547002 11.00000 -1.20000 AFIX 0 C22 1 0.835848 0.187372 0.450469 11.00000 0.01642 0.01630 = 0.01914 -0.00454 -0.00099 -0.00443 AFIX 43 H22 2 0.895969 0.129653 0.413560 11.00000 -1.20000 AFIX 0 C23 1 0.635969 0.477183 0.273577 11.00000 0.01561 0.01647 = 0.01514 -0.00322 0.00123 -0.00207 C24 1 0.549262 0.384761 0.280519 11.00000 0.02316 0.01910 = 0.02859 0.00197 -0.00416 -0.00705 AFIX 43 H24 2 0.587980 0.289131 0.305608 11.00000 -1.20000 AFIX 0 C25 1 0.407884 0.431422 0.251201 11.00000 0.02360 0.02887 = 0.03038 -0.00192 -0.00139 -0.01208 AFIX 43 H25 2 0.349496 0.368139 0.256841 11.00000 -1.20000 AFIX 0 C26 1 0.351087 0.569888 0.213685 11.00000 0.01567 0.02815 = 0.03052 -0.00773 -0.00236 -0.00187 AFIX 43 H26 2 0.254361 0.601516 0.192549 11.00000 -1.20000 AFIX 0 C27 1 0.435542 0.662114 0.207045 11.00000 0.02434 0.01860 = 0.03142 -0.00184 -0.00556 -0.00026 AFIX 43 H27 2 0.396190 0.757530 0.181721 11.00000 -1.20000 AFIX 0 C28 1 0.577546 0.616644 0.237062 11.00000 0.01932 0.01726 = 0.02194 -0.00333 0.00094 -0.00454 AFIX 43 H28 2 0.634613 0.681005 0.232589 11.00000 -1.20000 PART 1 21.000 AFIX 6 O1 4 0.528085 0.151255 -0.031412 21.00000 0.03124 0.03602 = 0.02466 -0.00197 -0.00103 0.00140 N5 3 0.343442 0.327943 0.003044 21.00000 0.03405 0.04109 = 0.03509 -0.01107 -0.01181 0.00019 C29 1 0.399960 0.203389 -0.019762 21.00000 0.03535 0.03833 = 0.02122 0.00192 -0.00029 -0.00736 H29 2 0.336830 0.150971 -0.027609 21.00000 -1.20000 C30 1 0.189033 0.385083 0.012808 21.00000 0.04027 0.05858 = 0.01922 0.02032 0.01397 0.01151 AFIX 137 H30A 2 0.139142 0.317167 0.000772 21.00000 -1.50000 H30B 2 0.155061 0.472880 -0.027773 21.00000 -1.50000 H30C 2 0.168445 0.403855 0.072029 21.00000 -1.50000 AFIX 5 C31 1 0.435958 0.415166 0.013767 21.00000 0.04033 0.04320 = 0.04478 -0.01787 -0.00944 0.00064 AFIX 137 H31A 2 0.487962 0.380617 0.068998 21.00000 -1.50000 H31B 2 0.377144 0.512361 0.013137 21.00000 -1.50000 H31C 2 0.505660 0.411812 -0.033545 21.00000 -1.50000 AFIX 6 PART 2 -21.000 O2 4 0.546665 0.160613 0.005200 -21.00000 0.02619 0.05138 = 0.04010 0.00426 -0.00974 -0.00835 N6 3 0.312209 0.282167 0.010751 -21.00000 0.02275 0.03981 = 0.03734 -0.01322 -0.00573 -0.00753 C32 1 0.450438 0.252845 0.030352 -21.00000 0.03989 0.04465 = 0.04234 0.01256 -0.01675 -0.02402 H32 2 0.476688 0.307024 0.066355 -21.00000 -1.20000 C33 1 0.203108 0.390566 0.045648 -21.00000 0.04420 0.04217 = 0.03621 0.02215 0.00001 -0.00610 AFIX 137 H33A 2 0.248054 0.428815 0.087467 -21.00000 -1.50000 H33B 2 0.128570 0.350172 0.074425 -21.00000 -1.50000 H33C 2 0.158899 0.466038 -0.001343 -21.00000 -1.50000 AFIX 5 C34 1 0.265105 0.198934 -0.042905 -21.00000 0.03407 0.06952 = 0.02861 -0.00134 -0.00334 -0.02329 AFIX 137 H34A 2 0.265823 0.241819 -0.103618 -21.00000 -1.50000 H34B 2 0.166836 0.194919 -0.026771 -21.00000 -1.50000 H34C 2 0.330636 0.103483 -0.034800 -21.00000 -1.50000 HKLF 4 REM sad in P-1 REM R1 = 0.0208 for 4821 Fo > 4sig(Fo) and 0.0223 for all 5094 data REM 399 parameters refined using 2 restraints END WGHT 0.0241 1.2665 REM Highest difference peak 0.333, deepest hole -0.537, 1-sigma level 0.057 Q1 1 0.8532 0.4998 0.3143 11.00000 0.05 0.33 Q2 1 0.3866 0.1756 -0.0334 11.00000 0.05 0.31 Q3 1 0.4604 0.2425 0.0555 11.00000 0.05 0.31 Q4 1 0.2777 0.3039 0.0339 11.00000 0.05 0.30 ; _database_code_depnum_ccdc_archive 'CCDC 939912' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[Pt(L)(PPh3)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H23 N4 P Pt S, 0.75(C H4 O)' _chemical_formula_sum 'C28.75 H26 N4 O0.75 P Pt S' _chemical_formula_weight 697.66 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' Pt Pt -1.7033 8.3905 '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 Trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 39.5689(12) _cell_length_b 39.5689(12) _cell_length_c 9.2324(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12518.5(7) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9854 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 30.12 _exptl_crystal_description block _exptl_crystal_colour RED _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6147 _exptl_absorpt_coefficient_mu 5.204 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.2953 _exptl_absorpt_correction_T_max 0.5983 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40144 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6380 _reflns_number_gt 5556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0281P)^2^+56.5045P] 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 6380 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _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 0.491054(4) 0.092807(4) 0.396947(13) 0.02872(5) Uani 1 1 d . . . S1 S 0.45215(3) 0.04724(3) 0.23454(11) 0.0394(2) Uani 1 1 d . . . P1 P 0.54482(2) 0.10715(2) 0.26816(9) 0.02653(17) Uani 1 1 d . . . N1 N 0.52158(9) 0.13101(9) 0.5596(3) 0.0351(6) Uani 1 1 d . . . N2 N 0.43883(9) 0.07917(9) 0.4948(3) 0.0396(7) Uani 1 1 d . . . N3 N 0.40384(9) 0.05021(10) 0.4365(4) 0.0452(8) Uani 1 1 d . . . N4 N 0.37574(11) 0.00571(11) 0.2523(5) 0.0569(10) Uani 1 1 d . . . H4A H 0.3802(15) -0.0004(15) 0.155(6) 0.068 Uiso 1 1 d . . . H4B H 0.3521(16) -0.0019(15) 0.292(5) 0.068 Uiso 1 1 d . . . C1 C 0.56088(12) 0.15113(13) 0.5915(4) 0.0439(9) Uani 1 1 d . . . H1 H 0.5801 0.1493 0.5359 0.053 Uiso 1 1 calc R . . C2 C 0.56906(14) 0.17389(13) 0.7120(4) 0.0497(10) Uani 1 1 d . . . H2 H 0.5940 0.1903 0.7534 0.060 Uiso 1 1 calc R . . C3 C 0.53294(14) 0.16818(12) 0.7624(4) 0.0474(10) Uani 1 1 d . . . C4 C 0.52155(18) 0.18282(14) 0.8794(5) 0.0629(14) Uani 1 1 d . . . H4 H 0.5405 0.2012 0.9443 0.076 Uiso 1 1 calc R . . C5 C 0.4828(2) 0.17022(16) 0.8987(5) 0.0744(17) Uani 1 1 d . . . H5 H 0.4751 0.1804 0.9773 0.089 Uiso 1 1 calc R . . C6 C 0.45461(17) 0.14344(15) 0.8083(5) 0.0653(14) Uani 1 1 d . . . H6 H 0.4280 0.1353 0.8262 0.078 Uiso 1 1 calc R . . C7 C 0.46452(13) 0.12755(13) 0.6880(4) 0.0478(10) Uani 1 1 d . . . C8 C 0.50422(12) 0.14116(12) 0.6660(4) 0.0404(9) Uani 1 1 d . . . C9 C 0.43455(13) 0.09791(13) 0.6052(4) 0.0489(11) Uani 1 1 d . . . H9 H 0.4086 0.0906 0.6314 0.059 Uiso 1 1 calc R . . C10 C 0.40763(11) 0.03456(11) 0.3188(5) 0.0442(9) Uani 1 1 d . . . C11 C 0.56236(11) 0.18479(10) 0.2712(4) 0.0340(7) Uani 1 1 d . . . H11 H 0.5405 0.1758 0.3340 0.041 Uiso 1 1 calc R . . C12 C 0.58330(12) 0.22398(11) 0.2317(4) 0.0426(9) Uani 1 1 d . . . H12 H 0.5756 0.2417 0.2669 0.051 Uiso 1 1 calc R . . C13 C 0.61532(13) 0.23709(11) 0.1412(4) 0.0469(9) Uani 1 1 d . . . H13 H 0.6299 0.2639 0.1156 0.056 Uiso 1 1 calc R . . C14 C 0.62613(12) 0.21126(11) 0.0880(4) 0.0443(9) Uani 1 1 d . . . H14 H 0.6481 0.2204 0.0259 0.053 Uiso 1 1 calc R . . C15 C 0.60501(10) 0.17197(10) 0.1248(4) 0.0361(8) Uani 1 1 d . . . H15 H 0.6122 0.1542 0.0859 0.043 Uiso 1 1 calc R . . C16 C 0.57335(10) 0.15868(9) 0.2187(3) 0.0293(7) Uani 1 1 d . . . C17 C 0.57529(10) 0.09257(11) 0.3668(4) 0.0330(7) Uani 1 1 d . . . C18 C 0.61559(10) 0.11449(12) 0.3752(4) 0.0386(8) Uani 1 1 d . . . H18 H 0.6292 0.1394 0.3302 0.046 Uiso 1 1 calc R . . C19 C 0.63587(12) 0.09997(14) 0.4496(4) 0.0499(10) Uani 1 1 d . . . H19 H 0.6634 0.1154 0.4582 0.060 Uiso 1 1 calc R . . C20 C 0.61665(14) 0.06346(16) 0.5115(5) 0.0583(13) Uani 1 1 d . . . H20 H 0.6310 0.0535 0.5598 0.070 Uiso 1 1 calc R . . C21 C 0.57682(14) 0.04150(15) 0.5033(5) 0.0587(12) Uani 1 1 d . . . H21 H 0.5635 0.0163 0.5460 0.070 Uiso 1 1 calc R . . C22 C 0.55586(12) 0.05615(12) 0.4326(5) 0.0469(10) Uani 1 1 d . . . H22 H 0.5282 0.0412 0.4293 0.056 Uiso 1 1 calc R . . C23 C 0.53737(10) 0.08249(10) 0.0946(4) 0.0328(7) Uani 1 1 d . . . C24 C 0.55051(12) 0.05635(12) 0.0690(5) 0.0461(9) Uani 1 1 d . . . H24 H 0.5642 0.0512 0.1424 0.055 Uiso 1 1 calc R . . C25 C 0.54357(15) 0.03794(14) -0.0633(5) 0.0620(13) Uani 1 1 d . . . H25 H 0.5524 0.0199 -0.0801 0.074 Uiso 1 1 calc R . . C26 C 0.52433(15) 0.04512(12) -0.1705(5) 0.0581(12) Uani 1 1 d . . . H26 H 0.5197 0.0321 -0.2610 0.070 Uiso 1 1 calc R . . C27 C 0.51170(16) 0.07119(13) -0.1474(4) 0.0614(13) Uani 1 1 d . . . H27 H 0.4985 0.0764 -0.2224 0.074 Uiso 1 1 calc R . . C28 C 0.51806(14) 0.08998(11) -0.0147(4) 0.0480(10) Uani 1 1 d . . . H28 H 0.5092 0.1080 0.0010 0.058 Uiso 1 1 calc R . . O1 O 0.33950(10) 0.04335(11) 0.5921(4) 0.0484(9) Uani 0.75 1 d P . . H1A H 0.3587 0.0457 0.5449 0.073 Uiso 0.75 1 calc PR . . C29 C 0.31837(19) 0.0541(2) 0.5081(8) 0.0655(17) Uani 0.75 1 d P . . H29A H 0.2911 0.0403 0.5401 0.098 Uiso 0.75 1 calc PR . . H29B H 0.3198 0.0474 0.4069 0.098 Uiso 0.75 1 calc PR . . H29C H 0.3290 0.0823 0.5164 0.098 Uiso 0.75 1 calc PR . . 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 0.02885(7) 0.03553(8) 0.02865(7) 0.00613(5) 0.00546(5) 0.02125(6) S1 0.0339(5) 0.0317(4) 0.0539(6) -0.0029(4) -0.0007(4) 0.0175(4) P1 0.0289(4) 0.0308(4) 0.0246(4) 0.0018(3) 0.0036(3) 0.0185(4) N1 0.0455(17) 0.0497(18) 0.0230(13) 0.0000(12) 0.0009(12) 0.0333(15) N2 0.0365(16) 0.0428(18) 0.0462(18) 0.0147(14) 0.0104(13) 0.0248(15) N3 0.0344(17) 0.051(2) 0.054(2) 0.0145(16) 0.0103(14) 0.0245(15) N4 0.0353(19) 0.049(2) 0.079(3) 0.006(2) -0.0010(19) 0.0157(17) C1 0.049(2) 0.064(3) 0.0322(19) -0.0070(17) -0.0076(16) 0.038(2) C2 0.068(3) 0.060(3) 0.033(2) -0.0082(18) -0.0134(19) 0.041(2) C3 0.078(3) 0.052(2) 0.0267(18) 0.0029(16) 0.0007(18) 0.043(2) C4 0.110(4) 0.058(3) 0.034(2) 0.0040(19) 0.015(2) 0.053(3) C5 0.122(5) 0.061(3) 0.049(3) 0.001(2) 0.033(3) 0.053(3) C6 0.084(4) 0.065(3) 0.066(3) 0.018(3) 0.040(3) 0.052(3) C7 0.065(3) 0.052(2) 0.041(2) 0.0132(18) 0.0201(19) 0.041(2) C8 0.060(2) 0.051(2) 0.0283(17) 0.0123(15) 0.0139(16) 0.042(2) C9 0.053(2) 0.061(3) 0.052(2) 0.024(2) 0.0308(19) 0.044(2) C10 0.0300(18) 0.035(2) 0.065(3) 0.0158(18) -0.0004(17) 0.0148(16) C11 0.0414(19) 0.0384(19) 0.0252(16) -0.0027(13) -0.0005(14) 0.0222(16) C12 0.059(2) 0.0359(19) 0.038(2) -0.0045(15) 0.0003(17) 0.0273(19) C13 0.057(3) 0.0304(19) 0.044(2) 0.0003(16) 0.0015(18) 0.0150(18) C14 0.042(2) 0.041(2) 0.039(2) 0.0029(16) 0.0096(16) 0.0128(17) C15 0.0390(19) 0.0352(18) 0.0339(18) -0.0014(14) 0.0060(14) 0.0185(16) C16 0.0330(17) 0.0307(17) 0.0260(15) -0.0015(12) -0.0017(13) 0.0173(14) C17 0.0356(18) 0.045(2) 0.0293(16) 0.0034(14) 0.0060(14) 0.0282(16) C18 0.0340(18) 0.056(2) 0.0336(18) 0.0014(16) 0.0034(14) 0.0279(18) C19 0.043(2) 0.081(3) 0.040(2) 0.002(2) 0.0006(17) 0.042(2) C20 0.066(3) 0.101(4) 0.044(2) 0.017(2) 0.008(2) 0.068(3) C21 0.068(3) 0.076(3) 0.059(3) 0.030(2) 0.020(2) 0.057(3) C22 0.044(2) 0.055(2) 0.056(2) 0.0209(19) 0.0157(18) 0.035(2) C23 0.0379(18) 0.0269(16) 0.0297(17) 0.0013(13) 0.0081(14) 0.0133(14) C24 0.048(2) 0.045(2) 0.051(2) -0.0088(18) 0.0037(18) 0.0271(19) C25 0.075(3) 0.054(3) 0.061(3) -0.020(2) 0.009(2) 0.035(3) C26 0.081(3) 0.038(2) 0.036(2) -0.0063(17) 0.015(2) 0.015(2) C27 0.101(4) 0.045(2) 0.028(2) 0.0017(17) -0.007(2) 0.029(3) C28 0.081(3) 0.038(2) 0.0329(19) 0.0004(16) -0.0039(19) 0.036(2) O1 0.0331(19) 0.050(2) 0.059(2) -0.0042(18) 0.0097(16) 0.0180(17) C29 0.051(4) 0.068(4) 0.072(4) -0.019(3) -0.006(3) 0.026(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 N1 2.043(3) . y Pt1 N2 2.065(3) . y Pt1 P1 2.2482(8) . y Pt1 S1 2.2567(10) . y S1 C10 1.754(4) . y P1 C17 1.819(3) . ? P1 C23 1.822(3) . ? P1 C16 1.827(3) . ? N1 C8 1.369(4) . ? N1 C1 1.379(5) . ? N2 C9 1.320(5) . y N2 N3 1.390(5) . y N3 C10 1.296(5) . y N4 C10 1.354(5) . y N4 H4A 0.97(5) . ? N4 H4B 0.90(5) . ? C1 C2 1.364(5) . ? C1 H1 0.9500 . ? C2 C3 1.410(6) . ? C2 H2 0.9500 . ? C3 C4 1.403(6) . ? C3 C8 1.418(6) . ? C4 C5 1.368(8) . ? C4 H4 0.9500 . ? C5 C6 1.371(8) . ? C5 H5 0.9500 . ? C6 C7 1.425(6) . ? C6 H6 0.9500 . ? C7 C8 1.398(6) . ? C7 C9 1.405(6) . ? C9 H9 0.9500 . ? C11 C12 1.392(5) . ? C11 C16 1.393(5) . ? C11 H11 0.9500 . ? C12 C13 1.384(6) . ? C12 H12 0.9500 . ? C13 C14 1.380(6) . ? C13 H13 0.9500 . ? C14 C15 1.390(5) . ? C14 H14 0.9500 . ? C15 C16 1.393(5) . ? C15 H15 0.9500 . ? C17 C18 1.385(5) . ? C17 C22 1.389(5) . ? C18 C19 1.381(5) . ? C18 H18 0.9500 . ? C19 C20 1.376(7) . ? C19 H19 0.9500 . ? C20 C21 1.369(7) . ? C20 H20 0.9500 . ? C21 C22 1.390(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.384(5) . ? C23 C24 1.391(5) . ? C24 C25 1.378(6) . ? C24 H24 0.9500 . ? C25 C26 1.362(7) . ? C25 H25 0.9500 . ? C26 C27 1.369(7) . ? C26 H26 0.9500 . ? C27 C28 1.389(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? O1 C29 1.355(8) . ? O1 H1A 0.8400 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N2 90.91(12) . . y N1 Pt1 P1 93.85(8) . . y N2 Pt1 P1 174.02(9) . . y N1 Pt1 S1 173.89(9) . . y N2 Pt1 S1 83.58(10) . . y P1 Pt1 S1 91.82(3) . . y C10 S1 Pt1 96.90(15) . . ? C17 P1 C23 103.05(16) . . ? C17 P1 C16 109.95(16) . . ? C23 P1 C16 102.84(15) . . ? C17 P1 Pt1 110.41(11) . . ? C23 P1 Pt1 116.79(12) . . ? C16 P1 Pt1 113.11(11) . . ? C8 N1 C1 105.3(3) . . ? C8 N1 Pt1 123.2(3) . . ? C1 N1 Pt1 131.6(2) . . ? C9 N2 N3 114.0(3) . . ? C9 N2 Pt1 125.7(3) . . ? N3 N2 Pt1 120.0(2) . . ? C10 N3 N2 114.4(3) . . ? C10 N4 H4A 115(3) . . ? C10 N4 H4B 118(3) . . ? H4A N4 H4B 125(4) . . ? C2 C1 N1 112.5(4) . . ? C2 C1 H1 123.8 . . ? N1 C1 H1 123.8 . . ? C1 C2 C3 106.0(4) . . ? C1 C2 H2 127.0 . . ? C3 C2 H2 127.0 . . ? C4 C3 C2 134.2(5) . . ? C4 C3 C8 119.5(4) . . ? C2 C3 C8 106.2(3) . . ? C5 C4 C3 118.9(5) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 122.2(4) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C7 121.3(5) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C9 124.0(4) . . ? C8 C7 C6 116.6(5) . . ? C9 C7 C6 119.3(4) . . ? N1 C8 C7 128.6(4) . . ? N1 C8 C3 110.0(3) . . ? C7 C8 C3 121.4(4) . . ? N2 C9 C7 126.6(4) . . ? N2 C9 H9 116.7 . . ? C7 C9 H9 116.7 . . ? N3 C10 N4 120.1(4) . . ? N3 C10 S1 125.1(3) . . ? N4 C10 S1 114.8(4) . . ? C12 C11 C16 120.2(3) . . ? C12 C11 H11 119.9 . . ? C16 C11 H11 119.9 . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.1(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 119.9(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 119.5(3) . . ? C11 C16 P1 119.6(3) . . ? C15 C16 P1 120.9(3) . . ? C18 C17 C22 119.5(3) . . ? C18 C17 P1 124.6(3) . . ? C22 C17 P1 115.9(3) . . ? C19 C18 C17 119.6(4) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 120.8(4) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 120.0(4) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 119.9(4) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 C21 120.2(4) . . ? C17 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C28 C23 C24 119.1(3) . . ? C28 C23 P1 119.0(3) . . ? C24 C23 P1 121.8(3) . . ? C25 C24 C23 119.6(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 C24 121.2(4) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 119.8(4) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C28 120.3(4) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C23 C28 C27 120.0(4) . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C29 O1 H1A 109.5 . . ? O1 C29 H29A 109.5 . . ? O1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C27 H27 Cg1 0.95 2.85 3.382(5) 117 1_554 C15 H15 Cg2 0.95 2.91 3.647(5) 135 18_545 N4 H4A O1 0.97(5) 2.14(5) 3.044(6) 154(4) 6_554 N4 H4B O1 0.90(5) 2.16(5) 2.939(5) 144(4) 8_544 O1 H1A N3 0.84 1.98 2.816(5) 178.6 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.009 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.096 loop_ _shelx_res_file ; TITL [Pt(L)(PPh3)] CELL 0.71073 39.5689 39.5689 9.2324 90.000 90.000 120.000 ZERR 18.00 0.0012 0.0012 0.0003 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H N O P Pt S UNIT 517.50 468 72 13.5 18 18 18 OMIT -1 2 0 OMIT -2 55 size 0.31 0.11 0.11 L.S. 24 ACTA BOND $H PLAN 0 TEMP -173 WGHT 0.028100 56.504501 FVAR 0.02341 PT1 6 0.491054 0.092807 0.396947 11.00000 0.02885 0.03553 = 0.02865 0.00613 0.00546 0.02125 S1 7 0.452148 0.047245 0.234543 11.00000 0.03393 0.03168 = 0.05392 -0.00286 -0.00073 0.01748 P1 5 0.544819 0.107148 0.268162 11.00000 0.02891 0.03077 = 0.02463 0.00182 0.00355 0.01846 N1 3 0.521579 0.131007 0.559563 11.00000 0.04549 0.04966 = 0.02295 -0.00002 0.00090 0.03334 N2 3 0.438834 0.079170 0.494820 11.00000 0.03647 0.04276 = 0.04621 0.01474 0.01043 0.02477 N3 3 0.403844 0.050214 0.436517 11.00000 0.03444 0.05098 = 0.05438 0.01454 0.01030 0.02446 N4 3 0.375743 0.005706 0.252272 11.00000 0.03532 0.04926 = 0.07894 0.00621 -0.00101 0.01574 H4A 2 0.380179 -0.000448 0.154650 11.00000 -1.20000 H4B 2 0.352118 -0.001915 0.292001 11.00000 -1.20000 C1 1 0.560883 0.151133 0.591530 11.00000 0.04896 0.06369 = 0.03218 -0.00699 -0.00755 0.03790 AFIX 43 H1 2 0.580122 0.149344 0.535874 11.00000 -1.20000 AFIX 0 C2 1 0.569062 0.173894 0.711954 11.00000 0.06831 0.06000 = 0.03317 -0.00824 -0.01336 0.04138 AFIX 43 H2 2 0.594031 0.190272 0.753434 11.00000 -1.20000 AFIX 0 C3 1 0.532939 0.168182 0.762373 11.00000 0.07818 0.05189 = 0.02669 0.00287 0.00072 0.04338 C4 1 0.521546 0.182824 0.879437 11.00000 0.11027 0.05817 = 0.03441 0.00403 0.01517 0.05268 AFIX 43 H4 2 0.540457 0.201189 0.944270 11.00000 -1.20000 AFIX 0 C5 1 0.482751 0.170216 0.898655 11.00000 0.12241 0.06071 = 0.04933 0.00148 0.03294 0.05275 AFIX 43 H5 2 0.475055 0.180352 0.977268 11.00000 -1.20000 AFIX 0 C6 1 0.454608 0.143444 0.808280 11.00000 0.08394 0.06524 = 0.06590 0.01788 0.04001 0.05161 AFIX 43 H6 2 0.427978 0.135330 0.826213 11.00000 -1.20000 AFIX 0 C7 1 0.464522 0.127554 0.687979 11.00000 0.06543 0.05183 = 0.04137 0.01323 0.02008 0.04063 C8 1 0.504224 0.141156 0.665986 11.00000 0.05996 0.05146 = 0.02834 0.01229 0.01392 0.04171 C9 1 0.434552 0.097909 0.605202 11.00000 0.05291 0.06133 = 0.05249 0.02374 0.03076 0.04360 AFIX 43 H9 2 0.408559 0.090610 0.631356 11.00000 -1.20000 AFIX 0 C10 1 0.407631 0.034562 0.318843 11.00000 0.02999 0.03536 = 0.06526 0.01576 -0.00042 0.01476 C11 1 0.562363 0.184790 0.271152 11.00000 0.04137 0.03844 = 0.02525 -0.00273 -0.00050 0.02217 AFIX 43 H11 2 0.540529 0.175843 0.333992 11.00000 -1.20000 AFIX 0 C12 1 0.583303 0.223978 0.231689 11.00000 0.05895 0.03590 = 0.03768 -0.00452 0.00035 0.02731 AFIX 43 H12 2 0.575622 0.241697 0.266863 11.00000 -1.20000 AFIX 0 C13 1 0.615323 0.237085 0.141151 11.00000 0.05708 0.03040 = 0.04407 0.00031 0.00150 0.01497 AFIX 43 H13 2 0.629887 0.263904 0.115558 11.00000 -1.20000 AFIX 0 C14 1 0.626126 0.211264 0.088002 11.00000 0.04229 0.04091 = 0.03909 0.00294 0.00961 0.01281 AFIX 43 H14 2 0.648127 0.220400 0.025903 11.00000 -1.20000 AFIX 0 C15 1 0.605010 0.171966 0.124788 11.00000 0.03901 0.03521 = 0.03386 -0.00136 0.00603 0.01849 AFIX 43 H15 2 0.612166 0.154198 0.085897 11.00000 -1.20000 AFIX 0 C16 1 0.573346 0.158676 0.218739 11.00000 0.03295 0.03069 = 0.02601 -0.00149 -0.00175 0.01727 C17 1 0.575288 0.092572 0.366785 11.00000 0.03557 0.04474 = 0.02935 0.00344 0.00605 0.02817 C18 1 0.615587 0.114494 0.375244 11.00000 0.03403 0.05557 = 0.03359 0.00144 0.00341 0.02785 AFIX 43 H18 2 0.629197 0.139377 0.330153 11.00000 -1.20000 AFIX 0 C19 1 0.635868 0.099971 0.449604 11.00000 0.04307 0.08140 = 0.03958 0.00188 0.00057 0.04198 AFIX 43 H19 2 0.663431 0.115379 0.458155 11.00000 -1.20000 AFIX 0 C20 1 0.616648 0.063460 0.511464 11.00000 0.06568 0.10078 = 0.04380 0.01666 0.00839 0.06822 AFIX 43 H20 2 0.631013 0.053485 0.559819 11.00000 -1.20000 AFIX 0 C21 1 0.576822 0.041500 0.503349 11.00000 0.06824 0.07631 = 0.05898 0.03022 0.02010 0.05671 AFIX 43 H21 2 0.563538 0.016284 0.546007 11.00000 -1.20000 AFIX 0 C22 1 0.555860 0.056153 0.432612 11.00000 0.04434 0.05456 = 0.05553 0.02089 0.01572 0.03511 AFIX 43 H22 2 0.528180 0.041225 0.429277 11.00000 -1.20000 AFIX 0 C23 1 0.537369 0.082489 0.094606 11.00000 0.03787 0.02688 = 0.02965 0.00126 0.00805 0.01327 C24 1 0.550512 0.056352 0.069039 11.00000 0.04765 0.04509 = 0.05062 -0.00881 0.00371 0.02705 AFIX 43 H24 2 0.564191 0.051217 0.142361 11.00000 -1.20000 AFIX 0 C25 1 0.543569 0.037941 -0.063338 11.00000 0.07523 0.05396 = 0.06099 -0.02044 0.00924 0.03539 AFIX 43 H25 2 0.552362 0.019908 -0.080140 11.00000 -1.20000 AFIX 0 C26 1 0.524331 0.045124 -0.170538 11.00000 0.08079 0.03810 = 0.03585 -0.00630 0.01482 0.01512 AFIX 43 H26 2 0.519700 0.032096 -0.261008 11.00000 -1.20000 AFIX 0 C27 1 0.511695 0.071189 -0.147406 11.00000 0.10087 0.04491 = 0.02809 0.00165 -0.00710 0.02875 AFIX 43 H27 2 0.498523 0.076442 -0.222392 11.00000 -1.20000 AFIX 0 C28 1 0.518063 0.089980 -0.014716 11.00000 0.08081 0.03831 = 0.03290 0.00040 -0.00395 0.03569 AFIX 43 H28 2 0.509168 0.107974 0.001011 11.00000 -1.20000 AFIX 0 O1 4 0.339496 0.043349 0.592148 10.75000 0.03307 0.04990 = 0.05863 -0.00418 0.00966 0.01796 AFIX 147 H1A 2 0.358709 0.045719 0.544919 10.75000 -1.50000 AFIX 0 C29 1 0.318372 0.054084 0.508080 10.75000 0.05145 0.06816 = 0.07208 -0.01886 -0.00610 0.02620 AFIX 137 H29A 2 0.291110 0.040341 0.540148 10.75000 -1.50000 H29B 2 0.319776 0.047372 0.406935 10.75000 -1.50000 H29C 2 0.328954 0.082303 0.516364 10.75000 -1.50000 HKLF 4 REM 4215_0m in R-3 REM R1 = 0.0248 for 5556 Fo > 4sig(Fo) and 0.0319 for all 6380 data REM 342 parameters refined using 0 restraints END WGHT 0.0282 56.4743 REM Highest difference peak 2.009, deepest hole -0.978, 1-sigma level 0.096 Q1 1 0.4901 0.0815 0.3297 11.00000 0.05 2.01 Q2 1 0.3272 0.0339 0.3879 11.00000 0.05 1.21 Q3 1 0.3266 0.0611 0.6472 11.00000 0.05 0.95 Q4 1 0.4614 0.0475 0.1559 11.00000 0.05 0.92 ; # start Validation Reply Form _vrf_PLAT601_ALERT_2_A ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 264 A**3 RESPONSE: ... There is no evidence for included solvent within the voids. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 939913'