# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Furukawa, Shuhei' _publ_contact_author_email shuhei.furukawa@kip.jst.go.jp loop_ _publ_author_name N.Louvain Y.Takashima S.Kitagawa S.Furukawa data_1 _database_code_depnum_ccdc_archive 'CCDC 809756' #TrackingRef '- 1_ccdc_deposit.cif' _audit_creation_date 2011-04-06T14:38:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Tris-ethylenediamine cadmium(II) bis-biphenyldithiolate cadmium(II) ethylenediamine ; _chemical_name_common ; Tris-ethylenediamine cadmium(ii) bis-biphenyldithiolate cadmium(ii) ethylenediamine ; _chemical_formula_moiety 'C24 H16 Cd S4, C6 H24 Cd N6, C2 H8 N2' _chemical_formula_analytical 'C32 H48 Cd2 N8 S4' _chemical_formula_sum 'C32 H48 Cd2 N8 S4' _chemical_formula_weight 897.869 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbc21 _symmetry_space_group_name_Hall 'P 2c -2b' _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, z' 'x, -y+1/2, z+1/2' _cell_length_a 9.1429(12) _cell_length_b 19.388(3) _cell_length_c 21.699(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3846.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 93.15 _cell_measurement_reflns_used 10835 _cell_measurement_theta_min 2.2276 _cell_measurement_theta_max 25.0479 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.365 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details ; ABSORPTION CORRECTION (EMPIRICAL) R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38. ; _exptl_absorpt_correction_T_min 0.8194 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 93.15 _diffrn_source_power 2.0000 _diffrn_source_voltage 50.0000 _diffrn_source_current 40.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 28.5714 _diffrn_orient_matrix_type d*Trek _diffrn_orient_matrix_ub_11 -0.0908 _diffrn_orient_matrix_ub_12 0.0557 _diffrn_orient_matrix_ub_13 0.025 _diffrn_orient_matrix_ub_21 0.0285 _diffrn_orient_matrix_ub_22 0.0415 _diffrn_orient_matrix_ub_23 0.0112 _diffrn_orient_matrix_ub_31 -0.0034 _diffrn_orient_matrix_ub_32 0.0141 _diffrn_orient_matrix_ub_33 -0.0437 _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_unetI/netI 0.0225 _diffrn_reflns_number 24811 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 6072 _reflns_number_gt 5756 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process 'Lp corrections applied' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SIR92 (Sirware)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. One neutral ethylenediamine molecule (en, H2N-CH2-CH2-NH2) is located in the "organic part" of the structure, i.e. located between [Cd(en)3]2+ cations. The presence of only one molecule per unit cell has been confirmed by elemental analysis (Anal. calc. for C32 H44 N8 S4 Cd2: C, 42.8; H, 5.4; N, 12.5. Found: C, 42.7; H, 5.5; N, 12.5). Therefore, the s.o.f. of this neutral ethylenediamine molecule has been fixed to 1. The molecule is disordered over two positions, the s.o.f. having been refined as 0.37139 and 0.62861 for each position. Interatomic distances of the neutral ethylenediamine molecule have been restrained to be similar to interatomic distances of one of the coordinated ethylenediamine ligand, in order to get a correct geometry thanks to the SADI command. The hydrogen atoms on the amine groups of the neutral molecule cannot be located by Fourier-difference, and were not included in the refinement but were taken into account for the molecular formula. ; _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^)+(0.0693P)^2^+4.3368P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6072 _refine_ls_number_parameters 410 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.43(3) _refine_diff_density_max 1.705 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.105 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0299(6) 0.5019(3) 0.3344(3) 0.0328(12) Uani 1 1 d . . . C2 C -0.0936(8) 0.4607(4) 0.3265(3) 0.0507(17) Uani 1 1 d . . . H2 H -0.1593 0.456 0.359 0.061 Uiso 1 1 calc R . . C3 C -0.1210(8) 0.4270(4) 0.2726(3) 0.0563(19) Uani 1 1 d . . . H3 H -0.204 0.3995 0.2698 0.068 Uiso 1 1 calc R . . C4 C -0.0302(7) 0.4322(3) 0.2220(3) 0.0364(13) Uani 1 1 d . . . C5 C 0.0953(8) 0.4720(3) 0.2290(3) 0.0441(15) Uani 1 1 d . . . H5 H 0.16 0.4762 0.1962 0.053 Uiso 1 1 calc R . . C6 C 0.1265(8) 0.5064(3) 0.2851(3) 0.0446(15) Uani 1 1 d . . . H6 H 0.2118 0.5322 0.289 0.053 Uiso 1 1 calc R . . C10 C -0.1162(6) 0.3235(3) 0.0507(3) 0.0303(12) Uani 1 1 d . . . C9 C -0.1677(9) 0.3004(4) 0.1077(3) 0.0532(18) Uani 1 1 d . . . H9 H -0.2222 0.2599 0.1089 0.064 Uiso 1 1 calc R . . C8 C -0.1415(9) 0.3347(4) 0.1620(3) 0.056(2) Uani 1 1 d . . . H8 H -0.1781 0.3168 0.1987 0.067 Uiso 1 1 calc R . . C7 C -0.0621(7) 0.3953(3) 0.1634(3) 0.0360(13) Uani 1 1 d . . . C12 C -0.0076(7) 0.4181(3) 0.1066(3) 0.0421(14) Uani 1 1 d . . . H12 H 0.0489 0.458 0.1053 0.051 Uiso 1 1 calc R . . C11 C -0.0353(7) 0.3832(3) 0.0526(3) 0.0429(15) Uani 1 1 d . . . H11 H 0.0023 0.4006 0.016 0.051 Uiso 1 1 calc R . . C13 C 0.5296(6) 0.5570(3) 0.4864(3) 0.0367(13) Uani 1 1 d . . . C14 C 0.6644(6) 0.5247(3) 0.4962(3) 0.0377(13) Uani 1 1 d . . . H14 H 0.7406 0.5312 0.4684 0.045 Uiso 1 1 calc R . . C15 C 0.6845(6) 0.4831(3) 0.5469(3) 0.0380(13) Uani 1 1 d . . . H15 H 0.7751 0.4621 0.552 0.046 Uiso 1 1 calc R . . C16 C 0.5767(6) 0.4707(3) 0.5909(3) 0.0368(13) Uani 1 1 d . . . C17 C 0.4435(7) 0.5046(4) 0.5810(3) 0.0472(15) Uani 1 1 d . . . H17 H 0.3691 0.4993 0.6099 0.057 Uiso 1 1 calc R . . C18 C 0.4186(7) 0.5454(3) 0.5303(3) 0.0420(14) Uani 1 1 d . . . H18 H 0.3273 0.5657 0.5248 0.05 Uiso 1 1 calc R . . C22 C 0.6704(7) 0.3416(3) 0.7482(3) 0.0378(14) Uani 1 1 d . . . C23 C 0.5526(8) 0.3861(4) 0.7484(3) 0.0522(17) Uani 1 1 d . . . H23 H 0.4927 0.3879 0.783 0.063 Uiso 1 1 calc R . . C24 C 0.5212(8) 0.4284(4) 0.6985(3) 0.0509(17) Uani 1 1 d . . . H24 H 0.4425 0.4587 0.7006 0.061 Uiso 1 1 calc R . . C19 C 0.6055(6) 0.4260(3) 0.6454(3) 0.0374(13) Uani 1 1 d . . . C20 C 0.7243(8) 0.3798(4) 0.6448(4) 0.0507(18) Uani 1 1 d . . . H20 H 0.7818 0.3756 0.6096 0.061 Uiso 1 1 calc R . . C21 C 0.7553(7) 0.3412(4) 0.6952(4) 0.0485(18) Uani 1 1 d . . . H21 H 0.8378 0.3132 0.6943 0.058 Uiso 1 1 calc R . . C25 C 0.6028(6) 0.3622(3) 0.4112(4) 0.0474(17) Uani 1 1 d . . . H25A H 0.6963 0.3528 0.3918 0.057 Uiso 1 1 calc R . . H25B H 0.6215 0.3799 0.4523 0.057 Uiso 1 1 calc R . . C26 C 0.5210(7) 0.4157(3) 0.3741(3) 0.0458(15) Uani 1 1 d . . . H26A H 0.5793 0.4573 0.3708 0.055 Uiso 1 1 calc R . . H26B H 0.5027 0.3984 0.3329 0.055 Uiso 1 1 calc R . . C27 C 0.1712(9) 0.1996(4) 0.3479(4) 0.0582(19) Uani 1 1 d . . . H27A H 0.1088 0.1598 0.3417 0.07 Uiso 1 1 calc R . . H27B H 0.2653 0.1899 0.3291 0.07 Uiso 1 1 calc R . . C28 C 0.1019(10) 0.2631(4) 0.3165(4) 0.072(2) Uani 1 1 d . . . H28A H 0.0918 0.2546 0.2727 0.086 Uiso 1 1 calc R . . H28B H 0.0053 0.2712 0.3334 0.086 Uiso 1 1 calc R . . C29 C 0.0940(7) 0.4017(4) 0.5361(4) 0.0543(18) Uani 1 1 d D . . H29A H 0.0049 0.4119 0.5585 0.065 Uiso 1 1 calc R . . H29B H 0.1509 0.4438 0.5331 0.065 Uiso 1 1 calc R . . C30 C 0.1819(9) 0.3468(4) 0.5707(4) 0.0572(19) Uani 1 1 d D . . H30A H 0.2042 0.3634 0.6118 0.069 Uiso 1 1 calc R . . H30B H 0.1233 0.3053 0.5747 0.069 Uiso 1 1 calc R . . N1 N 0.5173(5) 0.2978(2) 0.4154(3) 0.0381(12) Uani 1 1 d . . . H1A H 0.5502 0.2721 0.4471 0.046 Uiso 1 1 calc R . . H1B H 0.528 0.2732 0.3805 0.046 Uiso 1 1 calc R . . N2 N 0.3822(5) 0.4313(2) 0.4047(3) 0.0540(14) Uani 1 1 d . . . H2A H 0.3241 0.4558 0.3794 0.065 Uiso 1 1 calc R . . H2B H 0.3982 0.4562 0.439 0.065 Uiso 1 1 calc R . . N3 N 0.1911(6) 0.2116(2) 0.4142(3) 0.0470(14) Uani 1 1 d . . . H3A H 0.2579 0.182 0.4292 0.056 Uiso 1 1 calc R . . H3B H 0.1061 0.2043 0.4341 0.056 Uiso 1 1 calc R . . N4 N 0.1921(7) 0.3229(3) 0.3263(3) 0.0548(16) Uani 1 1 d . . . H4A H 0.1411 0.3614 0.3177 0.066 Uiso 1 1 calc R . . H4B H 0.2705 0.3214 0.3012 0.066 Uiso 1 1 calc R . . N5 N 0.0578(5) 0.3768(3) 0.4744(3) 0.0441(13) Uani 1 1 d D . . H5A H 0.0283 0.4122 0.4507 0.053 Uiso 1 1 calc R . . H5B H -0.0155 0.3459 0.4766 0.053 Uiso 1 1 calc R . . N6 N 0.3166(7) 0.3304(3) 0.5391(3) 0.0558(16) Uani 1 1 d D . . H6A H 0.3515 0.2897 0.5525 0.067 Uiso 1 1 calc R . . H6B H 0.384 0.3631 0.5467 0.067 Uiso 1 1 calc R . . S1 S 0.06095(15) 0.53919(6) 0.40707(7) 0.0337(3) Uani 1 1 d . . . S2 S -0.15686(15) 0.27580(6) -0.01686(7) 0.0308(3) Uani 1 1 d . . . S3 S 0.50767(14) 0.60845(7) 0.42106(8) 0.0414(4) Uani 1 1 d . . . S4 S 0.72015(19) 0.28681(9) 0.80954(7) 0.0418(4) Uani 1 1 d . . . Cd1 Cd 0.24180(4) 0.636971(18) 0.40217(2) 0.02567(11) Uani 1 1 d . . . Cd2 Cd 0.26856(4) 0.32428(2) 0.43044(2) 0.03662(13) Uani 1 1 d . . . N7A N 0.4800(18) 0.2947(10) 0.0784(7) 0.132(4) Uiso 0.630(12) 1 d PD A 1 C31A C 0.3428(16) 0.3224(8) 0.0971(7) 0.081(4) Uiso 0.630(12) 1 d PD A 1 H31A H 0.2647 0.3021 0.0729 0.097 Uiso 0.630(12) 1 calc PR A 1 H31B H 0.3417 0.3719 0.0905 0.097 Uiso 0.630(12) 1 calc PR A 1 C32A C 0.319(2) 0.3057(13) 0.1682(8) 0.128(8) Uiso 0.630(12) 1 d PD A 1 H32A H 0.2318 0.3296 0.1817 0.154 Uiso 0.630(12) 1 calc PR A 1 H32B H 0.3007 0.2567 0.1721 0.154 Uiso 0.630(12) 1 calc PR A 1 N8A N 0.437(2) 0.3235(11) 0.2104(7) 0.132(4) Uiso 0.630(12) 1 d PD A 1 N7B N 0.407(3) 0.4079(9) 0.1341(13) 0.132(4) Uiso 0.370(12) 1 d PD A 2 C31B C 0.3368(19) 0.3395(8) 0.1367(9) 0.047(5) Uiso 0.370(12) 1 d PD A 2 H31C H 0.32 0.3228 0.0952 0.057 Uiso 0.370(12) 1 calc PR A 2 H31D H 0.2428 0.3434 0.1571 0.057 Uiso 0.370(12) 1 calc PR A 2 C32B C 0.4329(16) 0.2878(6) 0.1717(6) 0.030(4) Uiso 0.370(12) 1 d PD A 2 H32C H 0.3856 0.243 0.1723 0.036 Uiso 0.370(12) 1 calc PR A 2 H32D H 0.5262 0.283 0.1509 0.036 Uiso 0.370(12) 1 calc PR A 2 N8B N 0.457(4) 0.3122(15) 0.2364(9) 0.132(4) Uiso 0.370(12) 1 d PD 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 C1 0.029(3) 0.036(3) 0.033(3) -0.002(2) -0.003(2) -0.004(2) C2 0.043(4) 0.068(4) 0.042(4) -0.014(3) 0.010(3) -0.021(3) C3 0.038(4) 0.083(5) 0.048(4) -0.010(4) 0.001(3) -0.031(4) C4 0.036(3) 0.041(3) 0.032(3) -0.003(2) 0.001(3) -0.008(2) C5 0.052(4) 0.047(3) 0.033(3) -0.003(3) 0.002(3) -0.019(3) C6 0.051(4) 0.038(3) 0.045(4) -0.001(3) -0.003(3) -0.021(3) C10 0.031(3) 0.031(3) 0.029(3) 0.004(2) -0.004(2) -0.001(2) C9 0.071(5) 0.050(4) 0.038(4) -0.005(3) 0.010(3) -0.031(4) C8 0.076(5) 0.050(4) 0.042(4) -0.006(3) 0.021(4) -0.032(3) C7 0.039(3) 0.039(3) 0.030(3) -0.003(2) 0.001(3) -0.012(2) C12 0.050(4) 0.042(3) 0.034(3) 0.004(3) -0.005(3) -0.023(3) C11 0.053(4) 0.051(4) 0.024(3) 0.014(3) -0.005(3) -0.022(3) C13 0.027(3) 0.034(3) 0.049(4) -0.002(3) -0.003(3) 0.001(2) C14 0.022(3) 0.047(3) 0.044(4) 0.001(3) 0.004(2) 0.000(2) C15 0.023(3) 0.049(3) 0.041(3) -0.001(3) -0.009(3) 0.001(2) C16 0.030(3) 0.046(3) 0.035(3) -0.001(2) -0.012(3) -0.001(2) C17 0.037(3) 0.059(4) 0.045(4) 0.000(3) 0.008(3) -0.002(3) C18 0.029(3) 0.049(3) 0.048(4) 0.008(3) -0.004(3) 0.006(3) C22 0.042(4) 0.044(3) 0.027(3) -0.004(2) -0.007(3) -0.015(3) C23 0.044(4) 0.069(5) 0.043(4) 0.009(3) 0.000(3) -0.002(3) C24 0.038(4) 0.076(5) 0.038(4) 0.003(3) -0.004(3) 0.008(3) C19 0.034(3) 0.043(3) 0.035(3) -0.003(2) -0.004(3) -0.006(2) C20 0.064(5) 0.049(4) 0.040(4) 0.004(3) 0.009(3) 0.009(3) C21 0.051(4) 0.053(4) 0.041(4) 0.004(3) 0.007(3) 0.014(3) C25 0.030(3) 0.035(3) 0.078(5) -0.006(3) -0.008(3) -0.001(2) C26 0.038(3) 0.039(3) 0.061(4) 0.006(3) 0.007(3) -0.008(2) C27 0.054(4) 0.057(4) 0.063(5) -0.011(4) -0.017(4) 0.002(3) C28 0.070(5) 0.069(5) 0.076(6) 0.015(4) -0.021(5) -0.022(4) C29 0.043(4) 0.049(4) 0.070(5) -0.004(3) 0.012(4) 0.004(3) C30 0.050(4) 0.062(4) 0.059(5) -0.004(4) 0.016(4) 0.004(4) N1 0.038(3) 0.030(2) 0.047(3) 0.000(2) -0.004(2) -0.0012(19) N2 0.038(3) 0.034(2) 0.090(4) 0.007(3) 0.016(3) 0.004(2) N3 0.030(2) 0.044(3) 0.066(4) 0.003(3) 0.004(3) 0.000(2) N4 0.042(3) 0.063(4) 0.059(4) 0.013(3) -0.007(3) -0.003(3) N5 0.029(3) 0.033(2) 0.070(4) 0.005(2) 0.001(3) -0.003(2) N6 0.038(3) 0.059(4) 0.070(4) -0.002(3) -0.001(3) 0.008(3) S1 0.0369(7) 0.0307(6) 0.0335(7) -0.0060(6) 0.0053(6) -0.0058(5) S2 0.0356(7) 0.0295(6) 0.0273(7) 0.0028(5) -0.0035(6) 0.0007(5) S3 0.0260(7) 0.0426(7) 0.0556(10) 0.0123(7) 0.0010(7) 0.0002(6) S4 0.0561(10) 0.0417(8) 0.0276(8) -0.0030(6) -0.0038(7) 0.0011(7) Cd1 0.02704(19) 0.02401(18) 0.0260(2) -0.00218(16) 0.00138(18) 0.00065(12) Cd2 0.0313(2) 0.0299(2) 0.0487(3) 0.00335(19) 0.0047(3) 0.00145(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C6 1.390(9) . ? C1 C2 1.394(9) . ? C1 S1 1.757(6) . ? C2 C3 1.364(9) . ? C2 H2 0.93 . ? C3 C4 1.380(9) . ? C3 H3 0.93 . ? C4 C5 1.392(8) . ? C4 C7 1.487(8) . ? C5 C6 1.418(9) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C10 C11 1.373(8) . ? C10 C9 1.397(8) . ? C10 S2 1.773(6) . ? C9 C8 1.376(9) . ? C9 H9 0.93 . ? C8 C7 1.381(8) . ? C8 H8 0.93 . ? C7 C12 1.401(8) . ? C12 C11 1.375(9) . ? C12 H12 0.93 . ? C11 H11 0.93 . ? C13 C14 1.400(8) . ? C13 C18 1.409(9) . ? C13 S3 1.745(6) . ? C14 C15 1.375(9) . ? C14 H14 0.93 . ? C15 C16 1.393(9) . ? C15 H15 0.93 . ? C16 C17 1.400(9) . ? C16 C19 1.491(8) . ? C17 C18 1.375(9) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C22 C23 1.380(10) . ? C22 C21 1.386(10) . ? C22 S4 1.763(6) . ? C23 C24 1.389(10) . ? C23 H23 0.93 . ? C24 C19 1.387(9) . ? C24 H24 0.93 . ? C19 C20 1.408(9) . ? C20 C21 1.355(11) . ? C20 H20 0.93 . ? C21 H21 0.93 . ? C25 N1 1.477(7) . ? C25 C26 1.510(9) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 N2 1.463(8) . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C27 N3 1.469(10) . ? C27 C28 1.543(11) . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? C28 N4 1.438(10) . ? C28 H28A 0.97 . ? C28 H28B 0.97 . ? C29 N5 1.461(9) . ? C29 C30 1.530(10) . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C30 N6 1.446(10) . ? C30 H30A 0.97 . ? C30 H30B 0.97 . ? N1 Cd2 2.354(5) . ? N1 H1A 0.9 . ? N1 H1B 0.9 . ? N2 Cd2 2.386(5) . ? N2 H2A 0.9 . ? N2 H2B 0.9 . ? N3 Cd2 2.324(5) . ? N3 H3A 0.9 . ? N3 H3B 0.9 . ? N4 Cd2 2.366(7) . ? N4 H4A 0.9 . ? N4 H4B 0.9 . ? N5 Cd2 2.379(5) . ? N5 H5A 0.9 . ? N5 H5B 0.9 . ? N6 Cd2 2.401(7) . ? N6 H6A 0.9 . ? N6 H6B 0.9 . ? S1 Cd1 2.5177(13) . ? S2 Cd1 2.5593(14) 2_564 ? S3 Cd1 2.5265(14) . ? S4 Cd1 2.5188(17) 2_665 ? Cd1 S4 2.5189(17) 2_664 ? Cd1 S2 2.5593(14) 2_565 ? N7A C31A 1.423(15) . ? C31A C32A 1.591(16) . ? C31A H31A 0.97 . ? C31A H31B 0.97 . ? C32A N8A 1.456(16) . ? C32A H32A 0.97 . ? C32A H32B 0.97 . ? N7B C31B 1.472(16) . ? C31B C32B 1.534(15) . ? C31B H31C 0.97 . ? C31B H31D 0.97 . ? C32B N8B 1.498(17) . ? C32B H32C 0.97 . ? C32B H32D 0.97 . ? 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 C6 C1 C2 117.2(5) . . ? C6 C1 S1 124.2(4) . . ? C2 C1 S1 118.5(5) . . ? C3 C2 C1 121.9(6) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 122.6(6) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C3 C4 C5 116.6(6) . . ? C3 C4 C7 121.9(5) . . ? C5 C4 C7 121.5(5) . . ? C4 C5 C6 121.4(6) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 120.2(5) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C11 C10 C9 115.1(5) . . ? C11 C10 S2 125.3(4) . . ? C9 C10 S2 119.6(4) . . ? C8 C9 C10 123.0(6) . . ? C8 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? C9 C8 C7 121.4(6) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C7 C12 115.9(6) . . ? C8 C7 C4 122.0(5) . . ? C12 C7 C4 122.1(5) . . ? C11 C12 C7 121.8(5) . . ? C11 C12 H12 119.1 . . ? C7 C12 H12 119.1 . . ? C10 C11 C12 122.7(5) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C14 C13 C18 117.4(6) . . ? C14 C13 S3 118.8(5) . . ? C18 C13 S3 123.9(4) . . ? C15 C14 C13 120.1(6) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 123.7(5) . . ? C14 C15 H15 118.1 . . ? C16 C15 H15 118.1 . . ? C15 C16 C17 115.5(6) . . ? C15 C16 C19 121.3(5) . . ? C17 C16 C19 123.2(6) . . ? C18 C17 C16 122.4(6) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C17 C18 C13 120.9(6) . . ? C17 C18 H18 119.5 . . ? C13 C18 H18 119.5 . . ? C23 C22 C21 116.3(6) . . ? C23 C22 S4 125.1(5) . . ? C21 C22 S4 118.6(5) . . ? C22 C23 C24 121.8(7) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C19 C24 C23 120.9(7) . . ? C19 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C19 C20 117.3(6) . . ? C24 C19 C16 122.8(6) . . ? C20 C19 C16 119.9(6) . . ? C21 C20 C19 120.3(7) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 123.3(7) . . ? C20 C21 H21 118.3 . . ? C22 C21 H21 118.3 . . ? N1 C25 C26 110.6(5) . . ? N1 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? N2 C26 C25 109.3(6) . . ? N2 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? N2 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? N3 C27 C28 110.9(6) . . ? N3 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? N4 C28 C27 110.1(6) . . ? N4 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? N4 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? N5 C29 C30 109.8(6) . . ? N5 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? N5 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? N6 C30 C29 111.5(6) . . ? N6 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? N6 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108 . . ? C25 N1 Cd2 109.6(3) . . ? C25 N1 H1A 109.7 . . ? Cd2 N1 H1A 109.7 . . ? C25 N1 H1B 109.7 . . ? Cd2 N1 H1B 109.7 . . ? H1A N1 H1B 108.2 . . ? C26 N2 Cd2 107.7(3) . . ? C26 N2 H2A 110.2 . . ? Cd2 N2 H2A 110.2 . . ? C26 N2 H2B 110.2 . . ? Cd2 N2 H2B 110.2 . . ? H2A N2 H2B 108.5 . . ? C27 N3 Cd2 109.6(4) . . ? C27 N3 H3A 109.8 . . ? Cd2 N3 H3A 109.8 . . ? C27 N3 H3B 109.8 . . ? Cd2 N3 H3B 109.8 . . ? H3A N3 H3B 108.2 . . ? C28 N4 Cd2 108.6(5) . . ? C28 N4 H4A 110 . . ? Cd2 N4 H4A 110 . . ? C28 N4 H4B 110 . . ? Cd2 N4 H4B 110 . . ? H4A N4 H4B 108.3 . . ? C29 N5 Cd2 109.0(4) . . ? C29 N5 H5A 109.9 . . ? Cd2 N5 H5A 109.9 . . ? C29 N5 H5B 109.9 . . ? Cd2 N5 H5B 109.9 . . ? H5A N5 H5B 108.3 . . ? C30 N6 Cd2 108.8(5) . . ? C30 N6 H6A 109.9 . . ? Cd2 N6 H6A 109.9 . . ? C30 N6 H6B 109.9 . . ? Cd2 N6 H6B 109.9 . . ? H6A N6 H6B 108.3 . . ? C1 S1 Cd1 112.23(19) . . ? C10 S2 Cd1 106.64(17) . 2_564 ? C13 S3 Cd1 111.6(2) . . ? C22 S4 Cd1 106.6(2) . 2_665 ? S1 Cd1 S4 124.48(6) . 2_664 ? S1 Cd1 S3 117.40(5) . . ? S4 Cd1 S3 97.18(6) 2_664 . ? S1 Cd1 S2 105.62(5) . 2_565 ? S4 Cd1 S2 101.66(5) 2_664 2_565 ? S3 Cd1 S2 108.98(5) . 2_565 ? N3 Cd2 N1 93.93(17) . . ? N3 Cd2 N4 75.8(2) . . ? N1 Cd2 N4 98.7(2) . . ? N3 Cd2 N5 102.49(18) . . ? N1 Cd2 N5 158.66(18) . . ? N4 Cd2 N5 98.5(2) . . ? N3 Cd2 N2 156.1(2) . . ? N1 Cd2 N2 74.72(16) . . ? N4 Cd2 N2 85.1(2) . . ? N5 Cd2 N2 94.29(17) . . ? N3 Cd2 N6 104.5(2) . . ? N1 Cd2 N6 88.3(2) . . ? N4 Cd2 N6 173.0(2) . . ? N5 Cd2 N6 74.5(2) . . ? N2 Cd2 N6 96.2(2) . . ? N7A C31A C32A 108.5(11) . . ? N7A C31A H31A 110 . . ? C32A C31A H31A 110 . . ? N7A C31A H31B 110 . . ? C32A C31A H31B 110 . . ? H31A C31A H31B 108.4 . . ? N8A C32A C31A 117.5(12) . . ? N8A C32A H32A 107.9 . . ? C31A C32A H32A 107.9 . . ? N8A C32A H32B 107.9 . . ? C31A C32A H32B 107.9 . . ? H32A C32A H32B 107.2 . . ? N7B C31B C32B 111.1(12) . . ? N7B C31B H31C 109.4 . . ? C32B C31B H31C 109.4 . . ? N7B C31B H31D 109.4 . . ? C32B C31B H31D 109.4 . . ? H31C C31B H31D 108 . . ? N8B C32B C31B 110.0(12) . . ? N8B C32B H32C 109.7 . . ? C31B C32B H32C 109.7 . . ? N8B C32B H32D 109.7 . . ? C31B C32B H32D 109.7 . . ? H32C C32B H32D 108.2 . . ? 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 H1A S2 0.9 2.94 3.616(5) 133 4_655 N1 H1B S4 0.9 2.61 3.378(5) 143.7 4_554 N2 H2A S1 0.9 2.96 3.607(5) 130.1 . N3 H3A S3 0.9 2.58 3.407(5) 153.1 3_645 N3 H3B S2 0.9 2.66 3.524(5) 161.9 4 N4 H4B N8B 0.9 2.22 3.12(4) 176.4 . N4 H4B N8A 0.9 2.49 3.37(2) 164.6 . N5 H5A S1 0.9 2.65 3.471(5) 151.4 . N5 H5B S2 0.9 2.69 3.555(5) 160.5 4 N6 H6A N7A 0.9 2.09 2.97(2) 166.6 4 # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment '- 2_ccdc_deposit.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-04-06 at 17:08:53 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : shelxl old_ccdc_deposit 2 old_archive 2 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_2 _database_code_depnum_ccdc_archive 'CCDC 809757' #TrackingRef '- 2_ccdc_deposit.cif' _audit_creation_date 2011-04-06T17:08:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C66 H88 Cd4 N12 S8' _chemical_formula_analytical 'C33 H44 Cd2 N6 S4' _chemical_formula_sum 'C66 H88 Cd4 N12 S8' _chemical_formula_weight 1755.67 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3757(11) _cell_length_b 16.437(2) _cell_length_c 23.660(3) _cell_angle_alpha 87.968(3) _cell_angle_beta 83.848(3) _cell_angle_gamma 85.414(3) _cell_volume 3612.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 93.15 _cell_measurement_reflns_used 7867 _cell_measurement_theta_min 1.4958 _cell_measurement_theta_max 22.488 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1764 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.441 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details ; ABSORPTION CORRECTION (EMPIRICAL) R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38. ; _exptl_absorpt_correction_T_min 0.8542 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 93.15 _diffrn_source_power 2.0000 _diffrn_source_voltage 50.0000 _diffrn_source_current 40.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 28.5714 _diffrn_orient_matrix_type d*Trek _diffrn_orient_matrix_ub_11 0.1038 _diffrn_orient_matrix_ub_12 -0.0114 _diffrn_orient_matrix_ub_13 0.026 _diffrn_orient_matrix_ub_21 -0.0162 _diffrn_orient_matrix_ub_22 -0.0549 _diffrn_orient_matrix_ub_23 0.0212 _diffrn_orient_matrix_ub_31 0.0036 _diffrn_orient_matrix_ub_32 -0.0151 _diffrn_orient_matrix_ub_33 -0.0396 _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_number 19482 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 22.48 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 9279 _reflns_number_gt 8029 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process 'Lp corrections applied' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SIR92 (Sirware)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 hydrogen atoms of the free standing amine groups of the 1,3-propane- diamine molecule cannot be located by Fourier-difference, and cannot be satisfactorily modelled, and were not included in the refinement but were taken into account for the molecular formula. ; _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^)+(0.0238P)^2^+12.2438P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9279 _refine_ls_number_parameters 839 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.1 _refine_ls_restrained_S_all 1.1 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.88 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.096 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.5491(5) 0.1228(3) 0.3046(2) 0.0155(12) Uani 1 1 d . . . C2 C 1.4847(5) 0.1964(3) 0.3275(2) 0.0184(12) Uani 1 1 d . . . H2 H 1.4165 0.2269 0.3082 0.022 Uiso 1 1 calc R . . C3 C 1.5203(5) 0.2241(3) 0.3777(2) 0.0173(12) Uani 1 1 d . . . H3 H 1.4776 0.2737 0.3911 0.021 Uiso 1 1 calc R . . C4 C 1.6190(5) 0.1796(3) 0.4093(2) 0.0149(12) Uani 1 1 d . . . C5 C 1.6742(5) 0.1036(3) 0.3889(2) 0.0164(12) Uani 1 1 d . . . H5 H 1.7344 0.0703 0.4102 0.02 Uiso 1 1 calc R . . C6 C 1.6404(5) 0.0769(3) 0.3372(2) 0.0160(12) Uani 1 1 d . . . H6 H 1.6807 0.0266 0.3242 0.019 Uiso 1 1 calc R . . C7 C 1.6684(5) 0.2154(3) 0.4592(2) 0.0181(12) Uani 1 1 d . . . C8 C 1.6925(5) 0.2989(3) 0.4585(2) 0.0182(12) Uani 1 1 d . . . H8 H 1.6764 0.3309 0.4262 0.022 Uiso 1 1 calc R . . C9 C 1.7395(5) 0.3346(3) 0.5046(2) 0.0175(12) Uani 1 1 d . . . H9 H 1.7553 0.3898 0.5027 0.021 Uiso 1 1 calc R . . C10 C 1.7634(5) 0.2884(3) 0.5539(2) 0.0155(12) Uani 1 1 d . A . C11 C 1.7415(5) 0.2053(3) 0.5549(2) 0.0171(12) Uani 1 1 d . . . H11 H 1.7576 0.1734 0.5871 0.02 Uiso 1 1 calc R . . C12 C 1.6961(5) 0.1698(3) 0.5085(2) 0.0181(12) Uani 1 1 d . . . H12 H 1.6836 0.1142 0.5101 0.022 Uiso 1 1 calc R . . C13 C 1.6310(5) 0.2803(3) 0.0432(2) 0.0172(12) Uani 1 1 d . . . C14 C 1.5119(5) 0.3362(3) 0.0446(2) 0.0166(12) Uani 1 1 d . . . H14 H 1.4427 0.336 0.0759 0.02 Uiso 1 1 calc R . . C15 C 1.4942(5) 0.3920(3) 0.0006(2) 0.0160(12) Uani 1 1 d . . . H15 H 1.4124 0.4282 0.0025 0.019 Uiso 1 1 calc R . . C16 C 1.5956(5) 0.3955(3) -0.0464(2) 0.0152(12) Uani 1 1 d . . . C17 C 1.7172(5) 0.3415(3) -0.0475(2) 0.0195(12) Uani 1 1 d . . . H17 H 1.7879 0.3432 -0.0782 0.023 Uiso 1 1 calc R . . C18 C 1.7344(6) 0.2851(3) -0.0036(2) 0.0216(13) Uani 1 1 d . . . H18 H 1.8169 0.2494 -0.0052 0.026 Uiso 1 1 calc R . . C19 C 1.5734(6) 0.4562(3) -0.0935(2) 0.0179(12) Uani 1 1 d . . . C20 C 1.4366(6) 0.4781(3) -0.1093(2) 0.0210(13) Uani 1 1 d . . . H20 H 1.3582 0.4532 -0.0908 0.025 Uiso 1 1 calc R . . C21 C 1.4151(6) 0.5366(3) -0.1520(2) 0.0218(13) Uani 1 1 d . . . H21 H 1.3223 0.5504 -0.1614 0.026 Uiso 1 1 calc R . . C22 C 1.5295(6) 0.5750(3) -0.1812(2) 0.0170(12) Uani 1 1 d . . . C23 C 1.6669(6) 0.5518(3) -0.1659(2) 0.0188(12) Uani 1 1 d . . . H23 H 1.7457 0.5756 -0.1849 0.023 Uiso 1 1 calc R . . C24 C 1.6883(5) 0.4939(3) -0.1230(2) 0.0171(12) Uani 1 1 d . . . H24 H 1.7811 0.4799 -0.1137 0.021 Uiso 1 1 calc R . . C25 C 1.1821(5) 0.2676(3) 0.0862(2) 0.0194(12) Uani 1 1 d . B . C26 C 1.0909(6) 0.3343(3) 0.0736(2) 0.0208(13) Uani 1 1 d . . . H26 H 1.045 0.3663 0.1028 0.025 Uiso 1 1 calc R . . C27 C 1.0673(6) 0.3539(3) 0.0178(2) 0.0243(13) Uani 1 1 d . . . H27 H 1.006 0.3994 0.0104 0.029 Uiso 1 1 calc R . . C28 C 1.1313(5) 0.3083(3) -0.0272(2) 0.0189(12) Uani 1 1 d . . . C29 C 1.2259(6) 0.2413(3) -0.0140(2) 0.0217(13) Uani 1 1 d . . . H29 H 1.2721 0.2095 -0.0433 0.026 Uiso 1 1 calc R . . C30 C 1.2517(6) 0.2217(3) 0.0417(2) 0.0209(13) Uani 1 1 d . . . H30 H 1.3158 0.1775 0.0493 0.025 Uiso 1 1 calc R . . C31 C 1.1011(5) 0.3268(3) -0.0864(2) 0.0182(12) Uani 1 1 d . . . C32 C 1.0837(5) 0.4068(3) -0.1079(2) 0.0179(12) Uani 1 1 d . . . H32 H 1.0923 0.4501 -0.0845 0.021 Uiso 1 1 calc R . . C33 C 1.0540(5) 0.4230(3) -0.1636(2) 0.0164(12) Uani 1 1 d . . . H33 H 1.0442 0.4769 -0.1768 0.02 Uiso 1 1 calc R . . C34 C 1.0385(5) 0.3602(3) -0.2001(2) 0.0165(12) Uani 1 1 d . . . C35 C 1.0544(5) 0.2806(3) -0.1785(2) 0.0199(12) Uani 1 1 d . . . H35 H 1.0441 0.2374 -0.2017 0.024 Uiso 1 1 calc R . . C36 C 1.0853(5) 0.2646(3) -0.1232(2) 0.0203(12) Uani 1 1 d . . . H36 H 1.0959 0.2106 -0.1102 0.024 Uiso 1 1 calc R . . C37 C 1.2243(5) 0.1686(3) -0.4387(2) 0.0198(12) Uani 1 1 d . . . C38 C 1.1050(6) 0.1810(3) -0.4685(2) 0.0220(13) Uani 1 1 d . . . H38 H 1.0321 0.2202 -0.4565 0.026 Uiso 1 1 calc R . . C39 C 1.0921(5) 0.1361(3) -0.5160(2) 0.0202(12) Uani 1 1 d . . . H39 H 1.0093 0.1449 -0.5344 0.024 Uiso 1 1 calc R . . C40 C 1.1993(5) 0.0783(3) -0.5367(2) 0.0175(12) Uani 1 1 d . . . C41 C 1.3235(6) 0.0682(3) -0.5079(2) 0.0198(12) Uani 1 1 d . . . H41 H 1.399 0.0314 -0.5213 0.024 Uiso 1 1 calc R . . C42 C 1.3352(5) 0.1117(3) -0.4599(2) 0.0199(12) Uani 1 1 d . . . H42 H 1.418 0.1033 -0.4414 0.024 Uiso 1 1 calc R . . C43 C 1.1823(5) 0.0273(3) -0.5853(2) 0.0167(12) Uani 1 1 d . . . C44 C 1.0469(6) 0.0004(3) -0.5925(2) 0.0190(12) Uani 1 1 d . . . H44 H 0.9677 0.0163 -0.5671 0.023 Uiso 1 1 calc R . . C45 C 1.0299(6) -0.0494(3) -0.6370(2) 0.0181(12) Uani 1 1 d . . . H45 H 0.9388 -0.0651 -0.6416 0.022 Uiso 1 1 calc R . . C46 C 1.1470(5) -0.0764(3) -0.6751(2) 0.0166(12) Uani 1 1 d . . . C47 C 1.2814(5) -0.0491(3) -0.6681(2) 0.0165(12) Uani 1 1 d . . . H47 H 1.3608 -0.0651 -0.6933 0.02 Uiso 1 1 calc R . . C48 C 1.2974(5) 0.0015(3) -0.6241(2) 0.0163(12) Uani 1 1 d . . . H48 H 1.3879 0.0187 -0.6204 0.02 Uiso 1 1 calc R . . C49A C 1.6043(14) 0.2982(7) 0.8056(5) 0.020(4) Uiso 0.499(16) 1 d P A 1 H49A H 1.6171 0.309 0.8447 0.024 Uiso 0.499(16) 1 calc PR A 1 H49B H 1.6723 0.2535 0.7926 0.024 Uiso 0.499(16) 1 calc PR A 1 C50A C 1.4501(15) 0.2772(11) 0.8008(5) 0.016(3) Uiso 0.499(16) 1 d P A 1 H50A H 1.3894 0.3277 0.7994 0.019 Uiso 0.499(16) 1 calc PR A 1 H50B H 1.4167 0.2471 0.8351 0.019 Uiso 0.499(16) 1 calc PR A 1 C49B C 1.4936(16) 0.3176(8) 0.8113(5) 0.029(4) Uani 0.501(16) 1 d P A 2 H49C H 1.5148 0.3146 0.8506 0.035 Uiso 0.501(16) 1 calc PR A 2 H49D H 1.4029 0.3501 0.8098 0.035 Uiso 0.501(16) 1 calc PR A 2 C50B C 1.4754(13) 0.2326(10) 0.7928(5) 0.026(4) Uani 0.501(16) 1 d P A 2 H50C H 1.5683 0.202 0.7925 0.031 Uiso 0.501(16) 1 calc PR A 2 H50D H 1.4111 0.2076 0.822 0.031 Uiso 0.501(16) 1 calc PR A 2 C51 C 1.4275(7) 0.2221(4) 0.7441(3) 0.0386(16) Uani 1 1 d . . . C52 C 1.2836(6) 0.5251(3) 0.6701(2) 0.0245(13) Uani 1 1 d . A . H52A H 1.355 0.5646 0.6615 0.029 Uiso 1 1 calc R . . H52B H 1.1982 0.5532 0.6894 0.029 Uiso 1 1 calc R . . C53 C 1.2464(5) 0.4921(3) 0.6148(2) 0.0217(13) Uani 1 1 d . . . H53A H 1.1862 0.4472 0.6241 0.026 Uiso 1 1 calc R . . H53B H 1.1891 0.5347 0.5962 0.026 Uiso 1 1 calc R . . C54 C 1.3701(6) 0.4626(3) 0.5727(2) 0.0234(13) Uani 1 1 d . A . H54A H 1.3342 0.4532 0.5367 0.028 Uiso 1 1 calc R . . H54B H 1.4376 0.5045 0.5663 0.028 Uiso 1 1 calc R . . C55 C 1.7098(6) 0.5496(3) 0.6181(2) 0.0240(13) Uani 1 1 d . A . H55A H 1.6236 0.5831 0.6104 0.029 Uiso 1 1 calc R . . H55B H 1.7293 0.5096 0.5885 0.029 Uiso 1 1 calc R . . C56 C 1.8342(6) 0.6034(4) 0.6147(2) 0.0307(14) Uani 1 1 d . . . H56A H 1.8143 0.644 0.6439 0.037 Uiso 1 1 calc R . . H56B H 1.9203 0.5702 0.6227 0.037 Uiso 1 1 calc R . . C57 C 1.8631(7) 0.6467(4) 0.5578(3) 0.0424(17) Uani 1 1 d . . . H57A H 1.7771 0.6796 0.5494 0.051 Uiso 1 1 calc R . . H57B H 1.9389 0.6831 0.5597 0.051 Uiso 1 1 calc R . . C58 C 1.0954(6) 0.2096(3) 0.3085(2) 0.0190(12) Uani 1 1 d . . . H58A H 1.1533 0.2477 0.2859 0.023 Uiso 1 1 calc R . . H58B H 1.1278 0.2051 0.3461 0.023 Uiso 1 1 calc R . . C59 C 0.9391(6) 0.2431(4) 0.3134(2) 0.0275(14) Uani 1 1 d . . . H59A H 0.8805 0.2003 0.3296 0.033 Uiso 1 1 calc R . . H59B H 0.9275 0.2871 0.3401 0.033 Uiso 1 1 calc R . . C60 C 0.8804(6) 0.2748(3) 0.2592(2) 0.0234(13) Uani 1 1 d . . . H60A H 0.7915 0.3081 0.2688 0.028 Uiso 1 1 calc R . . H60B H 0.9486 0.3094 0.2387 0.028 Uiso 1 1 calc R . . C61 C 0.9405(6) 0.0287(3) 0.0762(2) 0.0258(13) Uani 1 1 d . . . H61A H 1.0263 -0.0085 0.0714 0.031 Uiso 1 1 calc R . . H61B H 0.9061 0.0388 0.0391 0.031 Uiso 1 1 calc R . . C62 C 0.8264(6) -0.0113(3) 0.1153(2) 0.0247(13) Uani 1 1 d . . . H62A H 0.7873 -0.0522 0.0941 0.03 Uiso 1 1 calc R . . H62B H 0.7488 0.0298 0.1257 0.03 Uiso 1 1 calc R . . C63 C 0.8744(6) -0.0517(3) 0.1695(2) 0.0224(13) Uani 1 1 d . . . H63A H 0.8045 -0.0894 0.1847 0.027 Uiso 1 1 calc R . . H63B H 0.9658 -0.083 0.1606 0.027 Uiso 1 1 calc R . . C64 C 1.3296(6) 0.0140(4) 0.1198(2) 0.0300(14) Uani 1 1 d . B . H64A H 1.3826 0.0626 0.1171 0.036 Uiso 1 1 calc R . . H64B H 1.2652 0.0188 0.0902 0.036 Uiso 1 1 calc R . . C65 C 1.4355(6) -0.0589(4) 0.1078(3) 0.0337(15) Uani 1 1 d . . . C66A C 1.3642(12) -0.1265(7) 0.0786(5) 0.034(3) Uani 0.525(9) 1 d P B 1 H66A H 1.3421 -0.1073 0.0411 0.041 Uiso 0.525(9) 1 calc PR B 1 H66B H 1.4304 -0.1748 0.0744 0.041 Uiso 0.525(9) 1 calc PR B 1 N12A N 1.2341(10) -0.1464(6) 0.1126(4) 0.038(3) Uani 0.525(9) 1 d P B 1 C66B C 1.4896(14) -0.0606(9) 0.0512(6) 0.041(4) Uani 0.475(9) 1 d P B 2 H66C H 1.5697 -0.1017 0.0458 0.049 Uiso 0.475(9) 1 calc PR B 2 H66D H 1.5242 -0.008 0.0391 0.049 Uiso 0.475(9) 1 calc PR B 2 N12B N 1.3707(13) -0.0802(7) 0.0158(5) 0.046(4) Uani 0.475(9) 1 d P B 2 N1 N 1.6246(6) 0.3663(3) 0.77186(19) 0.0338(13) Uani 1 1 d . . . N2 N 1.5245(5) 0.2467(3) 0.69359(19) 0.0238(11) Uani 1 1 d . A . H2A H 1.4905 0.2284 0.6626 0.029 Uiso 1 1 calc R . . H2B H 1.6113 0.22 0.6962 0.029 Uiso 1 1 calc R . . N3 N 1.3400(4) 0.4606(3) 0.70860(18) 0.0217(10) Uani 1 1 d . . . H3A H 1.2725 0.4247 0.7163 0.026 Uiso 1 1 calc R A . H3B H 1.3515 0.4838 0.7416 0.026 Uiso 1 1 calc R . . N4 N 1.4460(5) 0.3861(3) 0.59285(18) 0.0214(10) Uani 1 1 d . . . H4A H 1.513 0.3695 0.5646 0.026 Uiso 1 1 calc R A . H4B H 1.3817 0.348 0.5977 0.026 Uiso 1 1 calc R . . N5 N 1.6821(5) 0.5064(3) 0.67352(18) 0.0208(10) Uani 1 1 d . . . H5A H 1.631 0.5416 0.6976 0.025 Uiso 1 1 calc R A . H5B H 1.7674 0.4939 0.6871 0.025 Uiso 1 1 calc R . . N6 N 1.9059(6) 0.5897(4) 0.5118(2) 0.0512(17) Uani 1 1 d . . . N7 N 1.1184(5) 0.1286(3) 0.28205(18) 0.0214(10) Uani 1 1 d . . . H7A H 1.0712 0.093 0.3055 0.026 Uiso 1 1 calc R . . H7B H 1.2128 0.1127 0.2809 0.026 Uiso 1 1 calc R . . N8 N 0.8522(4) 0.2090(3) 0.22161(19) 0.0208(10) Uani 1 1 d . . . H8A H 0.8167 0.2327 0.1907 0.025 Uiso 1 1 calc R . . H8B H 0.7828 0.1803 0.24 0.025 Uiso 1 1 calc R . . N9 N 0.9785(5) 0.1073(3) 0.09813(17) 0.0197(10) Uani 1 1 d . . . H9A H 0.9018 0.1435 0.0959 0.024 Uiso 1 1 calc R . . H9B H 1.0501 0.1253 0.0737 0.024 Uiso 1 1 calc R . . N10 N 0.8901(5) 0.0076(3) 0.21310(18) 0.0198(10) Uani 1 1 d . . . H10A H 0.9199 -0.0205 0.2436 0.024 Uiso 1 1 calc R . . H10B H 0.802 0.0313 0.224 0.024 Uiso 1 1 calc R . . N11 N 1.2420(4) 0.0131(3) 0.1750(2) 0.0249(11) Uani 1 1 d . . . H11A H 1.3008 0.0173 0.2023 0.03 Uiso 1 1 calc R B . H11B H 1.2056 -0.036 0.18 0.03 Uiso 1 1 calc R . . S1 S 1.51647(14) 0.09230(8) 0.23648(5) 0.0177(3) Uani 1 1 d . . . S2 S 1.81883(14) 0.33864(8) 0.61193(5) 0.0176(3) Uani 1 1 d . . . S3 S 1.65271(15) 0.20222(9) 0.09545(6) 0.0241(3) Uani 1 1 d . . . S4 S 1.50052(14) 0.64934(8) -0.23547(5) 0.0195(3) Uani 1 1 d . . . S5 S 1.20495(14) 0.24267(8) 0.15871(5) 0.0188(3) Uani 1 1 d . . . S6 S 1.00086(15) 0.38552(8) -0.27045(5) 0.0193(3) Uani 1 1 d . . . S7 S 1.24115(15) 0.21991(9) -0.37585(6) 0.0284(4) Uani 1 1 d . . . S8 S 1.12884(15) -0.14483(8) -0.72976(6) 0.0203(3) Uani 1 1 d . . . Cd1 Cd 1.46969(4) 0.22613(2) 0.179129(15) 0.01600(11) Uani 1 1 d . . . Cd2 Cd 1.56069(4) 0.38618(2) 0.676674(16) 0.01664(11) Uani 1 1 d . A . Cd3 Cd 1.04890(4) 0.11473(2) 0.189950(16) 0.01651(11) Uani 1 1 d . B . Cd4 Cd 0.99436(4) 0.25743(2) -0.327388(16) 0.01639(11) 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 C1 0.014(3) 0.021(3) 0.012(3) 0.002(2) -0.002(2) -0.006(2) C2 0.018(3) 0.020(3) 0.017(3) 0.005(2) -0.001(2) 0.001(2) C3 0.021(3) 0.018(3) 0.012(3) -0.002(2) 0.000(2) 0.000(2) C4 0.016(3) 0.017(3) 0.013(3) 0.003(2) -0.004(2) -0.004(2) C5 0.014(3) 0.020(3) 0.014(3) 0.004(2) -0.003(2) 0.000(2) C6 0.013(3) 0.018(3) 0.016(3) 0.002(2) 0.000(2) -0.002(2) C7 0.014(3) 0.024(3) 0.015(3) 0.002(2) -0.002(2) 0.002(2) C8 0.020(3) 0.017(3) 0.016(3) 0.004(2) -0.002(2) 0.002(2) C9 0.020(3) 0.015(3) 0.017(3) 0.001(2) -0.004(2) 0.000(2) C10 0.010(3) 0.019(3) 0.018(3) -0.004(2) -0.001(2) 0.000(2) C11 0.017(3) 0.022(3) 0.011(3) 0.006(2) 0.000(2) 0.000(2) C12 0.016(3) 0.018(3) 0.020(3) 0.005(2) -0.003(2) -0.002(2) C13 0.017(3) 0.017(3) 0.017(3) -0.001(2) -0.001(2) -0.003(2) C14 0.016(3) 0.019(3) 0.015(3) -0.003(2) 0.001(2) -0.004(2) C15 0.014(3) 0.015(3) 0.021(3) -0.002(2) -0.005(2) -0.002(2) C16 0.015(3) 0.013(3) 0.018(3) -0.003(2) -0.001(2) -0.005(2) C17 0.017(3) 0.023(3) 0.017(3) -0.004(2) 0.003(2) -0.001(2) C18 0.017(3) 0.025(3) 0.022(3) 0.003(3) 0.000(2) 0.000(2) C19 0.021(3) 0.015(3) 0.017(3) -0.004(2) -0.001(2) -0.001(2) C20 0.020(3) 0.025(3) 0.018(3) 0.000(2) 0.003(2) -0.008(2) C21 0.017(3) 0.029(3) 0.020(3) -0.002(3) -0.006(2) -0.001(3) C22 0.024(3) 0.012(3) 0.016(3) -0.004(2) -0.004(2) 0.001(2) C23 0.018(3) 0.018(3) 0.021(3) 0.000(2) 0.001(2) -0.007(2) C24 0.012(3) 0.017(3) 0.023(3) -0.005(2) -0.005(2) 0.003(2) C25 0.016(3) 0.022(3) 0.020(3) 0.008(2) -0.004(2) -0.006(2) C26 0.024(3) 0.021(3) 0.018(3) -0.004(2) -0.005(2) 0.000(3) C27 0.025(3) 0.026(3) 0.023(3) 0.003(3) -0.007(3) 0.000(3) C28 0.018(3) 0.024(3) 0.015(3) 0.002(2) -0.006(2) -0.003(2) C29 0.020(3) 0.028(3) 0.017(3) 0.000(2) -0.001(2) -0.004(3) C30 0.017(3) 0.026(3) 0.020(3) 0.004(2) -0.005(2) -0.001(2) C31 0.012(3) 0.026(3) 0.018(3) 0.002(2) -0.004(2) -0.003(2) C32 0.013(3) 0.024(3) 0.017(3) -0.005(2) -0.004(2) -0.003(2) C33 0.013(3) 0.017(3) 0.020(3) 0.002(2) -0.005(2) 0.001(2) C34 0.011(3) 0.025(3) 0.014(3) 0.000(2) -0.003(2) -0.003(2) C35 0.021(3) 0.021(3) 0.019(3) -0.002(2) -0.005(2) -0.004(2) C36 0.020(3) 0.020(3) 0.022(3) 0.003(2) -0.006(2) -0.001(2) C37 0.017(3) 0.018(3) 0.024(3) 0.003(2) 0.003(2) -0.007(2) C38 0.018(3) 0.020(3) 0.027(3) 0.002(3) 0.003(3) -0.001(2) C39 0.013(3) 0.026(3) 0.022(3) 0.001(2) -0.007(2) -0.002(2) C40 0.015(3) 0.019(3) 0.019(3) 0.007(2) -0.001(2) -0.006(2) C41 0.017(3) 0.017(3) 0.025(3) 0.001(2) 0.000(2) 0.000(2) C42 0.012(3) 0.021(3) 0.027(3) -0.004(2) -0.006(2) -0.002(2) C43 0.016(3) 0.013(3) 0.021(3) 0.008(2) -0.004(2) -0.002(2) C44 0.018(3) 0.020(3) 0.018(3) 0.009(2) -0.001(2) 0.003(2) C45 0.015(3) 0.018(3) 0.022(3) 0.006(2) -0.005(2) -0.003(2) C46 0.020(3) 0.011(3) 0.018(3) 0.005(2) -0.005(2) 0.001(2) C47 0.017(3) 0.016(3) 0.015(3) 0.005(2) 0.000(2) 0.001(2) C48 0.013(3) 0.017(3) 0.018(3) 0.006(2) -0.002(2) -0.003(2) C49B 0.042(10) 0.028(8) 0.018(7) -0.006(5) 0.008(6) -0.017(7) C50B 0.028(7) 0.017(9) 0.031(8) -0.005(6) 0.012(6) 0.000(6) C51 0.038(4) 0.030(4) 0.045(4) -0.006(3) 0.012(3) -0.011(3) C52 0.022(3) 0.021(3) 0.030(3) 0.001(3) -0.004(3) 0.000(3) C53 0.015(3) 0.024(3) 0.027(3) 0.006(2) -0.007(2) -0.002(2) C54 0.023(3) 0.028(3) 0.021(3) 0.003(2) -0.006(2) -0.004(3) C55 0.022(3) 0.016(3) 0.033(3) 0.000(3) 0.001(3) 0.000(2) C56 0.030(3) 0.032(4) 0.031(3) -0.008(3) 0.003(3) -0.012(3) C57 0.041(4) 0.037(4) 0.051(4) 0.007(3) 0.002(3) -0.023(3) C58 0.028(3) 0.015(3) 0.015(3) 0.001(2) -0.006(2) -0.004(2) C59 0.026(3) 0.033(3) 0.024(3) -0.015(3) 0.004(3) -0.007(3) C60 0.016(3) 0.022(3) 0.033(3) -0.007(3) -0.007(3) 0.002(2) C61 0.028(3) 0.031(3) 0.019(3) -0.006(3) -0.009(3) 0.002(3) C62 0.025(3) 0.019(3) 0.032(3) -0.006(3) -0.013(3) -0.002(3) C63 0.022(3) 0.018(3) 0.029(3) -0.004(2) -0.008(3) -0.001(2) C64 0.033(3) 0.032(4) 0.027(3) -0.007(3) -0.014(3) 0.004(3) C65 0.025(3) 0.029(4) 0.048(4) -0.013(3) -0.003(3) 0.002(3) C66A 0.021(6) 0.031(7) 0.050(8) -0.009(6) 0.000(6) -0.004(5) N12A 0.035(6) 0.038(6) 0.040(6) -0.006(5) 0.001(5) -0.002(5) C66B 0.028(8) 0.037(9) 0.054(10) -0.009(7) 0.002(7) 0.016(6) N12B 0.061(8) 0.053(8) 0.028(7) -0.026(6) -0.020(6) 0.004(6) N1 0.053(3) 0.034(3) 0.015(3) -0.004(2) -0.013(2) 0.007(3) N2 0.019(2) 0.019(3) 0.034(3) -0.004(2) -0.003(2) 0.002(2) N3 0.019(2) 0.026(3) 0.020(3) -0.005(2) -0.004(2) 0.000(2) N4 0.019(2) 0.029(3) 0.017(2) -0.006(2) -0.003(2) 0.001(2) N5 0.017(2) 0.021(3) 0.024(3) -0.003(2) 0.000(2) -0.004(2) N6 0.053(4) 0.080(5) 0.024(3) -0.011(3) 0.003(3) -0.038(3) N7 0.028(3) 0.017(2) 0.020(3) 0.0022(19) -0.009(2) -0.001(2) N8 0.015(2) 0.019(2) 0.028(3) -0.004(2) -0.002(2) 0.000(2) N9 0.017(2) 0.023(3) 0.019(2) -0.003(2) -0.002(2) -0.003(2) N10 0.020(2) 0.019(2) 0.021(2) 0.001(2) -0.007(2) 0.002(2) N11 0.014(2) 0.018(3) 0.043(3) 0.000(2) -0.007(2) -0.004(2) S1 0.0203(7) 0.0180(7) 0.0155(7) 0.0015(6) -0.0050(6) -0.0032(6) S2 0.0180(7) 0.0194(7) 0.0156(7) -0.0017(6) -0.0042(6) -0.0001(6) S3 0.0237(8) 0.0245(8) 0.0214(8) 0.0076(6) 0.0015(6) 0.0050(6) S4 0.0241(7) 0.0181(7) 0.0169(7) 0.0009(6) -0.0068(6) -0.0010(6) S5 0.0155(7) 0.0245(8) 0.0169(7) 0.0038(6) -0.0032(6) -0.0044(6) S6 0.0255(8) 0.0190(7) 0.0146(7) 0.0005(6) -0.0068(6) -0.0035(6) S7 0.0160(7) 0.0348(9) 0.0357(9) -0.0167(7) -0.0018(7) -0.0043(6) S8 0.0253(8) 0.0187(7) 0.0177(7) 0.0017(6) -0.0049(6) -0.0038(6) Cd1 0.0167(2) 0.0181(2) 0.0137(2) 0.00163(16) -0.00377(16) -0.00244(16) Cd2 0.0171(2) 0.0172(2) 0.0161(2) -0.00030(16) -0.00362(16) -0.00196(16) Cd3 0.0160(2) 0.0173(2) 0.0167(2) -0.00231(16) -0.00381(16) -0.00081(16) Cd4 0.0167(2) 0.0168(2) 0.0162(2) -0.00045(16) -0.00392(16) -0.00193(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C6 1.375(7) . ? C1 C2 1.408(7) . ? C1 S1 1.770(5) . ? C2 C3 1.370(7) . ? C2 H2 0.93 . ? C3 C4 1.397(7) . ? C3 H3 0.93 . ? C4 C5 1.396(7) . ? C4 C7 1.471(7) . ? C5 C6 1.391(7) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C12 1.400(7) . ? C7 C8 1.407(7) . ? C8 C9 1.385(7) . ? C8 H8 0.93 . ? C9 C10 1.396(7) . ? C9 H9 0.93 . ? C10 C11 1.398(7) . ? C10 S2 1.772(5) . ? C11 C12 1.381(7) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.386(7) . ? C13 C18 1.396(7) . ? C13 S3 1.765(5) . ? C14 C15 1.378(7) . ? C14 H14 0.93 . ? C15 C16 1.387(7) . ? C15 H15 0.93 . ? C16 C17 1.386(7) . ? C16 C19 1.490(7) . ? C17 C18 1.383(7) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 C20 1.390(7) . ? C19 C24 1.395(7) . ? C20 C21 1.390(7) . ? C20 H20 0.93 . ? C21 C22 1.394(7) . ? C21 H21 0.93 . ? C22 C23 1.396(7) . ? C22 S4 1.768(5) . ? C23 C24 1.384(7) . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 C26 1.380(7) . ? C25 C30 1.391(8) . ? C25 S5 1.780(5) . ? C26 C27 1.386(7) . ? C26 H26 0.93 . ? C27 C28 1.379(8) . ? C27 H27 0.93 . ? C28 C29 1.405(7) . ? C28 C31 1.476(7) . ? C29 C30 1.389(7) . ? C29 H29 0.93 . ? C30 H30 0.93 . ? C31 C36 1.392(7) . ? C31 C32 1.398(7) . ? C32 C33 1.386(7) . ? C32 H32 0.93 . ? C33 C34 1.396(7) . ? C33 H33 0.93 . ? C34 C35 1.389(7) . ? C34 S6 1.767(5) . ? C35 C36 1.383(7) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C37 C38 1.383(7) . ? C37 C42 1.405(7) . ? C37 S7 1.762(5) . ? C38 C39 1.387(7) . ? C38 H38 0.93 . ? C39 C40 1.388(7) . ? C39 H39 0.93 . ? C40 C41 1.408(7) . ? C40 C43 1.475(7) . ? C41 C42 1.381(7) . ? C41 H41 0.93 . ? C42 H42 0.93 . ? C43 C48 1.390(7) . ? C43 C44 1.406(7) . ? C44 C45 1.387(7) . ? C44 H44 0.93 . ? C45 C46 1.398(7) . ? C45 H45 0.93 . ? C46 C47 1.399(7) . ? C46 S8 1.774(5) . ? C47 C48 1.382(7) . ? C47 H47 0.93 . ? C48 H48 0.93 . ? C49A N1 1.365(11) . ? C49A C50A 1.530(18) . ? C49A H49A 0.97 . ? C49A H49B 0.97 . ? C50A C51 1.687(16) . ? C50A H50A 0.97 . ? C50A H50B 0.97 . ? C49B C50B 1.51(2) . ? C49B N1 1.696(13) . ? C49B H49C 0.97 . ? C49B H49D 0.97 . ? C50B C51 1.302(13) . ? C50B H50C 0.97 . ? C50B H50D 0.97 . ? C51 N2 1.488(7) . ? C52 N3 1.475(7) . ? C52 C53 1.519(7) . ? C52 H52A 0.97 . ? C52 H52B 0.97 . ? C53 C54 1.507(7) . ? C53 H53A 0.97 . ? C53 H53B 0.97 . ? C54 N4 1.483(7) . ? C54 H54A 0.97 . ? C54 H54B 0.97 . ? C55 N5 1.478(7) . ? C55 C56 1.513(7) . ? C55 H55A 0.97 . ? C55 H55B 0.97 . ? C56 C57 1.509(8) . ? C56 H56A 0.97 . ? C56 H56B 0.97 . ? C57 N6 1.462(8) . ? C57 H57A 0.97 . ? C57 H57B 0.97 . ? C58 N7 1.481(6) . ? C58 C59 1.518(7) . ? C58 H58A 0.97 . ? C58 H58B 0.97 . ? C59 C60 1.507(8) . ? C59 H59A 0.97 . ? C59 H59B 0.97 . ? C60 N8 1.481(6) . ? C60 H60A 0.97 . ? C60 H60B 0.97 . ? C61 N9 1.492(7) . ? C61 C62 1.513(8) . ? C61 H61A 0.97 . ? C61 H61B 0.97 . ? C62 C63 1.519(8) . ? C62 H62A 0.97 . ? C62 H62B 0.97 . ? C63 N10 1.470(6) . ? C63 H63A 0.97 . ? C63 H63B 0.97 . ? C64 N11 1.466(7) . ? C64 C65 1.509(8) . ? C64 H64A 0.97 . ? C64 H64B 0.97 . ? C65 C66B 1.381(15) . ? C65 C66A 1.558(12) . ? C66A N12A 1.440(14) . ? C66A H66A 0.97 . ? C66A H66B 0.97 . ? C66B N12B 1.524(17) . ? C66B H66C 0.97 . ? C66B H66D 0.97 . ? N1 Cd2 2.396(4) . ? N2 Cd2 2.358(4) . ? N2 H2A 0.9 . ? N2 H2B 0.9 . ? N3 Cd2 2.382(4) . ? N3 H3A 0.9 . ? N3 H3B 0.9 . ? N4 Cd2 2.355(4) . ? N4 H4A 0.9 . ? N4 H4B 0.9 . ? N5 Cd2 2.353(4) . ? N5 H5A 0.9 . ? N5 H5B 0.9 . ? N7 Cd3 2.364(4) . ? N7 H7A 0.9 . ? N7 H7B 0.9 . ? N8 Cd3 2.386(4) . ? N8 H8A 0.9 . ? N8 H8B 0.9 . ? N9 Cd3 2.347(4) . ? N9 H9A 0.9 . ? N9 H9B 0.9 . ? N10 Cd3 2.407(4) . ? N10 H10A 0.9 . ? N10 H10B 0.9 . ? N11 Cd3 2.370(4) . ? N11 H11A 0.9 . ? N11 H11B 0.9 . ? S1 Cd1 2.5758(14) . ? S2 Cd4 2.5633(13) 1_656 ? S2 Cd2 2.7933(14) . ? S3 Cd1 2.4977(14) . ? S4 Cd1 2.5317(14) 2_865 ? S5 Cd1 2.5706(13) . ? S5 Cd3 2.6942(14) . ? S6 Cd4 2.5477(14) . ? S7 Cd4 2.5104(15) . ? S8 Cd4 2.5332(14) 2_754 ? Cd1 S4 2.5317(14) 2_865 ? Cd4 S8 2.5332(14) 2_754 ? Cd4 S2 2.5633(13) 1_454 ? 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 C6 C1 C2 116.9(5) . . ? C6 C1 S1 121.9(4) . . ? C2 C1 S1 121.3(4) . . ? C3 C2 C1 121.4(5) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 121.7(5) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 116.9(5) . . ? C5 C4 C7 122.7(4) . . ? C3 C4 C7 120.3(5) . . ? C6 C5 C4 121.0(5) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C1 C6 C5 121.9(5) . . ? C1 C6 H6 119 . . ? C5 C6 H6 119 . . ? C12 C7 C8 116.8(5) . . ? C12 C7 C4 123.1(5) . . ? C8 C7 C4 120.1(4) . . ? C9 C8 C7 121.7(5) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 120.6(5) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 118.2(5) . . ? C9 C10 S2 118.2(4) . . ? C11 C10 S2 123.5(4) . . ? C12 C11 C10 120.9(5) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C7 121.8(5) . . ? C11 C12 H12 119.1 . . ? C7 C12 H12 119.1 . . ? C14 C13 C18 117.2(5) . . ? C14 C13 S3 123.3(4) . . ? C18 C13 S3 119.4(4) . . ? C15 C14 C13 121.3(5) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 121.4(5) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C17 C16 C15 117.8(5) . . ? C17 C16 C19 121.9(5) . . ? C15 C16 C19 120.3(5) . . ? C18 C17 C16 120.7(5) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C13 121.5(5) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? C20 C19 C24 117.5(5) . . ? C20 C19 C16 121.0(5) . . ? C24 C19 C16 121.5(5) . . ? C19 C20 C21 121.1(5) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C22 121.5(5) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C21 C22 C23 117.1(5) . . ? C21 C22 S4 121.1(4) . . ? C23 C22 S4 121.8(4) . . ? C24 C23 C22 121.4(5) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C19 121.4(5) . . ? C23 C24 H24 119.3 . . ? C19 C24 H24 119.3 . . ? C26 C25 C30 118.6(5) . . ? C26 C25 S5 119.0(4) . . ? C30 C25 S5 122.4(4) . . ? C25 C26 C27 120.4(5) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 122.4(5) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 116.7(5) . . ? C27 C28 C31 122.5(5) . . ? C29 C28 C31 120.8(5) . . ? C30 C29 C28 121.3(5) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C25 120.4(5) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C36 C31 C32 116.8(5) . . ? C36 C31 C28 121.1(5) . . ? C32 C31 C28 122.0(5) . . ? C33 C32 C31 121.2(5) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 121.5(5) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C35 C34 C33 117.3(5) . . ? C35 C34 S6 123.8(4) . . ? C33 C34 S6 118.9(4) . . ? C36 C35 C34 121.1(5) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C31 122.0(5) . . ? C35 C36 H36 119 . . ? C31 C36 H36 119 . . ? C38 C37 C42 117.5(5) . . ? C38 C37 S7 123.0(4) . . ? C42 C37 S7 119.5(4) . . ? C37 C38 C39 121.3(5) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C38 C39 C40 121.9(5) . . ? C38 C39 H39 119.1 . . ? C40 C39 H39 119.1 . . ? C39 C40 C41 116.9(5) . . ? C39 C40 C43 121.9(5) . . ? C41 C40 C43 121.2(5) . . ? C42 C41 C40 121.2(5) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C41 C42 C37 121.2(5) . . ? C41 C42 H42 119.4 . . ? C37 C42 H42 119.4 . . ? C48 C43 C44 117.3(5) . . ? C48 C43 C40 122.5(4) . . ? C44 C43 C40 120.2(5) . . ? C45 C44 C43 120.9(5) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C46 121.2(5) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C45 C46 C47 117.8(5) . . ? C45 C46 S8 121.8(4) . . ? C47 C46 S8 120.5(4) . . ? C48 C47 C46 120.7(5) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C43 122.0(5) . . ? C47 C48 H48 119 . . ? C43 C48 H48 119 . . ? N1 C49A C50A 106.1(10) . . ? N1 C49A H49A 110.5 . . ? C50A C49A H49A 110.5 . . ? N1 C49A H49B 110.5 . . ? C50A C49A H49B 110.5 . . ? H49A C49A H49B 108.7 . . ? C49A C50A C51 115.5(10) . . ? C49A C50A H50A 108.4 . . ? C51 C50A H50A 108.4 . . ? C49A C50A H50B 108.4 . . ? C51 C50A H50B 108.4 . . ? H50A C50A H50B 107.5 . . ? C50B C49B N1 114.8(9) . . ? C50B C49B H49C 108.6 . . ? N1 C49B H49C 108.6 . . ? C50B C49B H49D 108.6 . . ? N1 C49B H49D 108.6 . . ? H49C C49B H49D 107.5 . . ? C51 C50B C49B 119.9(12) . . ? C51 C50B H50C 107.3 . . ? C49B C50B H50C 107.3 . . ? C51 C50B H50D 107.3 . . ? C49B C50B H50D 107.3 . . ? H50C C50B H50D 106.9 . . ? C50B C51 N2 114.6(7) . . ? C50B C51 C50A 26.3(6) . . ? N2 C51 C50A 110.7(6) . . ? N3 C52 C53 112.9(4) . . ? N3 C52 H52A 109 . . ? C53 C52 H52A 109 . . ? N3 C52 H52B 109 . . ? C53 C52 H52B 109 . . ? H52A C52 H52B 107.8 . . ? C54 C53 C52 117.1(4) . . ? C54 C53 H53A 108 . . ? C52 C53 H53A 108 . . ? C54 C53 H53B 108 . . ? C52 C53 H53B 108 . . ? H53A C53 H53B 107.3 . . ? N4 C54 C53 111.9(4) . . ? N4 C54 H54A 109.2 . . ? C53 C54 H54A 109.2 . . ? N4 C54 H54B 109.2 . . ? C53 C54 H54B 109.2 . . ? H54A C54 H54B 107.9 . . ? N5 C55 C56 114.0(5) . . ? N5 C55 H55A 108.7 . . ? C56 C55 H55A 108.7 . . ? N5 C55 H55B 108.7 . . ? C56 C55 H55B 108.7 . . ? H55A C55 H55B 107.6 . . ? C57 C56 C55 113.8(5) . . ? C57 C56 H56A 108.8 . . ? C55 C56 H56A 108.8 . . ? C57 C56 H56B 108.8 . . ? C55 C56 H56B 108.8 . . ? H56A C56 H56B 107.7 . . ? N6 C57 C56 112.3(5) . . ? N6 C57 H57A 109.1 . . ? C56 C57 H57A 109.1 . . ? N6 C57 H57B 109.1 . . ? C56 C57 H57B 109.1 . . ? H57A C57 H57B 107.9 . . ? N7 C58 C59 112.9(4) . . ? N7 C58 H58A 109 . . ? C59 C58 H58A 109 . . ? N7 C58 H58B 109 . . ? C59 C58 H58B 109 . . ? H58A C58 H58B 107.8 . . ? C60 C59 C58 116.8(5) . . ? C60 C59 H59A 108.1 . . ? C58 C59 H59A 108.1 . . ? C60 C59 H59B 108.1 . . ? C58 C59 H59B 108.1 . . ? H59A C59 H59B 107.3 . . ? N8 C60 C59 113.2(4) . . ? N8 C60 H60A 108.9 . . ? C59 C60 H60A 108.9 . . ? N8 C60 H60B 108.9 . . ? C59 C60 H60B 108.9 . . ? H60A C60 H60B 107.7 . . ? N9 C61 C62 112.8(4) . . ? N9 C61 H61A 109 . . ? C62 C61 H61A 109 . . ? N9 C61 H61B 109 . . ? C62 C61 H61B 109 . . ? H61A C61 H61B 107.8 . . ? C61 C62 C63 116.4(5) . . ? C61 C62 H62A 108.2 . . ? C63 C62 H62A 108.2 . . ? C61 C62 H62B 108.2 . . ? C63 C62 H62B 108.2 . . ? H62A C62 H62B 107.3 . . ? N10 C63 C62 112.6(4) . . ? N10 C63 H63A 109.1 . . ? C62 C63 H63A 109.1 . . ? N10 C63 H63B 109.1 . . ? C62 C63 H63B 109.1 . . ? H63A C63 H63B 107.8 . . ? N11 C64 C65 116.3(5) . . ? N11 C64 H64A 108.2 . . ? C65 C64 H64A 108.2 . . ? N11 C64 H64B 108.2 . . ? C65 C64 H64B 108.2 . . ? H64A C64 H64B 107.4 . . ? C66B C65 C64 111.5(7) . . ? C66B C65 C66A 71.5(8) . . ? C64 C65 C66A 110.6(6) . . ? N12A C66A C65 109.8(9) . . ? N12A C66A H66A 109.7 . . ? C65 C66A H66A 109.7 . . ? N12A C66A H66B 109.7 . . ? C65 C66A H66B 109.7 . . ? H66A C66A H66B 108.2 . . ? C65 C66B N12B 109.0(10) . . ? C65 C66B H66C 109.9 . . ? N12B C66B H66C 109.9 . . ? C65 C66B H66D 109.9 . . ? N12B C66B H66D 109.9 . . ? H66C C66B H66D 108.3 . . ? C49A N1 C49B 38.5(6) . . ? C49A N1 Cd2 125.7(5) . . ? C49B N1 Cd2 108.8(5) . . ? C51 N2 Cd2 119.1(3) . . ? C51 N2 H2A 107.5 . . ? Cd2 N2 H2A 107.5 . . ? C51 N2 H2B 107.5 . . ? Cd2 N2 H2B 107.5 . . ? H2A N2 H2B 107 . . ? C52 N3 Cd2 117.5(3) . . ? C52 N3 H3A 107.9 . . ? Cd2 N3 H3A 107.9 . . ? C52 N3 H3B 107.9 . . ? Cd2 N3 H3B 107.9 . . ? H3A N3 H3B 107.2 . . ? C54 N4 Cd2 119.5(3) . . ? C54 N4 H4A 107.4 . . ? Cd2 N4 H4A 107.4 . . ? C54 N4 H4B 107.4 . . ? Cd2 N4 H4B 107.4 . . ? H4A N4 H4B 107 . . ? C55 N5 Cd2 118.3(3) . . ? C55 N5 H5A 107.7 . . ? Cd2 N5 H5A 107.7 . . ? C55 N5 H5B 107.7 . . ? Cd2 N5 H5B 107.7 . . ? H5A N5 H5B 107.1 . . ? C58 N7 Cd3 118.9(3) . . ? C58 N7 H7A 107.6 . . ? Cd3 N7 H7A 107.6 . . ? C58 N7 H7B 107.6 . . ? Cd3 N7 H7B 107.6 . . ? H7A N7 H7B 107 . . ? C60 N8 Cd3 117.8(3) . . ? C60 N8 H8A 107.8 . . ? Cd3 N8 H8A 107.8 . . ? C60 N8 H8B 107.8 . . ? Cd3 N8 H8B 107.8 . . ? H8A N8 H8B 107.2 . . ? C61 N9 Cd3 121.2(3) . . ? C61 N9 H9A 107 . . ? Cd3 N9 H9A 107 . . ? C61 N9 H9B 107 . . ? Cd3 N9 H9B 107 . . ? H9A N9 H9B 106.8 . . ? C63 N10 Cd3 118.9(3) . . ? C63 N10 H10A 107.6 . . ? Cd3 N10 H10A 107.6 . . ? C63 N10 H10B 107.6 . . ? Cd3 N10 H10B 107.6 . . ? H10A N10 H10B 107 . . ? C64 N11 Cd3 117.6(3) . . ? C64 N11 H11A 107.9 . . ? Cd3 N11 H11A 107.9 . . ? C64 N11 H11B 107.9 . . ? Cd3 N11 H11B 107.9 . . ? H11A N11 H11B 107.2 . . ? C1 S1 Cd1 105.29(17) . . ? C10 S2 Cd4 117.24(17) . 1_656 ? C10 S2 Cd2 103.74(16) . . ? Cd4 S2 Cd2 111.30(5) 1_656 . ? C13 S3 Cd1 110.13(18) . . ? C22 S4 Cd1 97.48(16) . 2_865 ? C25 S5 Cd1 113.54(17) . . ? C25 S5 Cd3 107.46(17) . . ? Cd1 S5 Cd3 115.77(5) . . ? C34 S6 Cd4 110.96(18) . . ? C37 S7 Cd4 108.82(18) . . ? C46 S8 Cd4 100.61(17) . 2_754 ? S3 Cd1 S4 114.96(5) . 2_865 ? S3 Cd1 S5 116.54(5) . . ? S4 Cd1 S5 103.98(4) 2_865 . ? S3 Cd1 S1 99.78(4) . . ? S4 Cd1 S1 112.08(4) 2_865 . ? S5 Cd1 S1 109.67(4) . . ? N5 Cd2 N4 107.00(15) . . ? N5 Cd2 N2 157.39(15) . . ? N4 Cd2 N2 90.44(16) . . ? N5 Cd2 N3 90.51(15) . . ? N4 Cd2 N3 80.91(15) . . ? N2 Cd2 N3 106.72(15) . . ? N5 Cd2 N1 86.33(16) . . ? N4 Cd2 N1 164.78(17) . . ? N2 Cd2 N1 78.74(16) . . ? N3 Cd2 N1 91.88(16) . . ? N5 Cd2 S2 78.37(11) . . ? N4 Cd2 S2 88.08(11) . . ? N2 Cd2 S2 88.19(11) . . ? N3 Cd2 S2 161.40(11) . . ? N1 Cd2 S2 102.11(13) . . ? N9 Cd3 N7 177.47(15) . . ? N9 Cd3 N11 94.32(16) . . ? N7 Cd3 N11 87.53(16) . . ? N9 Cd3 N8 94.19(15) . . ? N7 Cd3 N8 84.12(15) . . ? N11 Cd3 N8 170.16(16) . . ? N9 Cd3 N10 84.34(14) . . ? N7 Cd3 N10 97.44(14) . . ? N11 Cd3 N10 88.50(15) . . ? N8 Cd3 N10 87.42(15) . . ? N9 Cd3 S5 91.72(11) . . ? N7 Cd3 S5 86.37(11) . . ? N11 Cd3 S5 96.08(11) . . ? N8 Cd3 S5 88.60(11) . . ? N10 Cd3 S5 174.18(11) . . ? S7 Cd4 S8 116.56(5) . 2_754 ? S7 Cd4 S6 109.20(5) . . ? S8 Cd4 S6 112.74(5) 2_754 . ? S7 Cd4 S2 116.13(5) . 1_454 ? S8 Cd4 S2 110.68(4) 2_754 1_454 ? S6 Cd4 S2 88.11(4) . 1_454 ? 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 N2 H2A S7 0.9 2.61 3.336(5) 137.8 1_556 N2 H2B S8 0.9 2.82 3.704(5) 167.5 2_855 N3 H3A S6 0.9 2.66 3.483(5) 152.3 1_556 N4 H4B S7 0.9 2.6 3.477(5) 166.8 1_556 N5 H5A S4 0.9 2.56 3.463(5) 175.7 1_556 N5 H5B S6 0.9 2.95 3.788(5) 156 1_656 N7 H7B S1 0.9 2.92 3.778(5) 158.9 . N8 H8A S3 0.9 2.94 3.698(4) 143.1 1_455 N8 H8B S1 0.9 2.99 3.794(4) 149 1_455 N9 H9A S3 0.9 2.46 3.322(5) 161.7 1_455 N10 H10A S8 0.9 2.82 3.554(4) 139.8 1_556 N10 H10B S1 0.9 2.77 3.657(4) 168.1 1_455 N11 H11A S1 0.9 2.66 3.451(4) 146.9 . N11 H11B N12A 0.9 2.44 3.064(11) 126.8 . N11 H11B S8 0.9 2.81 3.529(5) 138.2 1_556 # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment '- 3_ccdc_deposit.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-04-07 at 02:25:00 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : shelxl old_ccdc_deposit 3 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_3 _database_code_depnum_ccdc_archive 'CCDC 809758' #TrackingRef '- 3_ccdc_deposit.cif' _audit_creation_date 2011-04-07T02:25:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; N,N-diethyl-1,3-propanediamine biphenyldithiolate cadmium(II) ; _chemical_formula_moiety 'C19 H26 Cd N2 S2' _chemical_formula_analytical 'C19 H26 Cd N2 S2' _chemical_formula_sum 'C19 H26 Cd N2 S2' _chemical_formula_weight 458.97 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2439(3) _cell_length_b 21.1076(9) _cell_length_c 22.4715(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3910.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 93.15 _cell_measurement_reflns_used 8338 _cell_measurement_theta_min 1.3236 _cell_measurement_theta_max 25.025 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.334 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details ; ABSORPTION CORRECTION (EMPIRICAL) R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38. ; _exptl_absorpt_correction_T_min 0.8648 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 93.15 _diffrn_source_power 2.0000 _diffrn_source_voltage 50.0000 _diffrn_source_current 40.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 28.5714 _diffrn_orient_matrix_type d*Trek _diffrn_orient_matrix_ub_11 -0.1181 _diffrn_orient_matrix_ub_12 0.0127 _diffrn_orient_matrix_ub_13 -0.0244 _diffrn_orient_matrix_ub_21 0.01 _diffrn_orient_matrix_ub_22 0.0038 _diffrn_orient_matrix_ub_23 -0.0462 _diffrn_orient_matrix_ub_31 -0.0038 _diffrn_orient_matrix_ub_32 -0.0441 _diffrn_orient_matrix_ub_33 -0.0044 _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_unetI/netI 0.0143 _diffrn_reflns_number 31077 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 3431 _reflns_number_gt 3089 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process 'Lp corrections applied' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SIR92 (Sirware)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0340P)^2^+3.3043P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_number_reflns 3431 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.032 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0657 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.628 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.09 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8111(3) 0.23495(11) 0.82176(11) 0.0161(5) Uani 1 1 d . . . C2 C 0.9389(3) 0.27768(12) 0.82787(12) 0.0189(5) Uani 1 1 d . . . C3 C 0.9630(3) 0.30919(13) 0.88117(12) 0.0201(6) Uani 1 1 d . . . C4 C 0.8599(3) 0.30039(12) 0.93020(11) 0.0163(5) Uani 1 1 d . . . C5 C 0.7340(3) 0.25638(12) 0.92337(11) 0.0176(5) Uani 1 1 d . . . C6 C 0.7102(3) 0.22471(12) 0.87046(11) 0.0172(5) Uani 1 1 d . . . C7 C 0.8827(3) 0.33661(11) 0.98610(11) 0.0164(5) Uani 1 1 d . . . C8 C 0.9675(3) 0.39421(13) 0.98690(12) 0.0175(5) Uani 1 1 d . . . C9 C 0.9937(3) 0.42710(12) 1.03910(12) 0.0187(6) Uani 1 1 d . . . C10 C 0.9349(3) 0.40490(12) 1.09360(11) 0.0169(5) Uani 1 1 d . . . C11 C 0.8454(3) 0.34851(12) 1.09284(11) 0.0174(5) Uani 1 1 d . . . C12 C 0.8211(3) 0.31509(12) 1.04049(11) 0.0169(5) Uani 1 1 d . . . C13 C 0.4445(3) 0.08521(14) 0.62553(12) 0.0210(6) Uani 1 1 d . . . C14 C 0.4439(4) 0.03656(13) 0.57579(12) 0.0225(6) Uani 1 1 d . . . C15 C 0.3845(3) -0.02880(13) 0.59563(12) 0.0224(6) Uani 1 1 d . . . C16 C 0.4152(4) -0.10879(14) 0.67345(13) 0.0257(6) Uani 1 1 d . . . C17 C 0.3139(5) -0.08096(18) 0.72349(15) 0.0344(7) Uani 1 1 d . . . C18 C 0.6414(3) -0.08474(13) 0.60709(14) 0.0243(6) Uani 1 1 d . . . C19 C 0.6138(4) -0.14214(14) 0.56701(14) 0.0278(6) Uani 1 1 d . . . N1 N 0.5569(3) 0.06920(11) 0.67510(10) 0.0179(5) Uani 1 1 d . . . N2 N 0.4960(3) -0.05985(10) 0.63763(10) 0.0203(5) Uani 1 1 d . . . S1 S 0.78043(7) 0.19691(3) 0.75201(3) 0.01528(15) Uani 1 1 d . . . S2 S 0.97169(8) 0.45026(3) 1.15856(3) 0.01673(15) Uani 1 1 d . . . Cd1 Cd 0.53060(2) 0.125182(8) 0.759660(8) 0.01500(8) Uani 1 1 d . . . H1A H 0.546(3) 0.0289(16) 0.6837(13) 0.022(8) Uiso 1 1 d . . . H1B H 0.657(4) 0.0734(14) 0.6635(14) 0.031(9) Uiso 1 1 d . . . H2 H 1.007(3) 0.2852(13) 0.7955(14) 0.021(7) Uiso 1 1 d . . . H3 H 1.050(4) 0.3402(15) 0.8855(14) 0.031(8) Uiso 1 1 d . . . H3A H 0.337(4) 0.0868(13) 0.6424(13) 0.022(7) Uiso 1 1 d . . . H5 H 0.658(4) 0.2475(13) 0.9550(13) 0.021(7) Uiso 1 1 d . . . H6 H 0.621(3) 0.1965(12) 0.8678(11) 0.014(7) Uiso 1 1 d . . . H8 H 1.008(3) 0.4124(14) 0.9512(14) 0.021(7) Uiso 1 1 d . . . H9 H 1.055(3) 0.4675(13) 1.0363(12) 0.019(7) Uiso 1 1 d . . . H11 H 0.803(3) 0.3306(12) 1.1268(12) 0.011(6) Uiso 1 1 d . . . H12 H 0.762(4) 0.2786(14) 1.0430(12) 0.021(7) Uiso 1 1 d . . . H13B H 0.473(4) 0.1289(15) 0.6114(17) 0.037(10) Uiso 1 1 d . . . H14A H 0.371(4) 0.0506(13) 0.5434(13) 0.022(7) Uiso 1 1 d . . . H14B H 0.554(4) 0.0333(13) 0.5562(13) 0.020(7) Uiso 1 1 d . . . H15A H 0.283(3) -0.0234(12) 0.6165(12) 0.015(7) Uiso 1 1 d . . . H15B H 0.365(3) -0.0565(13) 0.5616(12) 0.016(7) Uiso 1 1 d . . . H16A H 0.498(4) -0.1353(15) 0.6883(16) 0.031(9) Uiso 1 1 d . . . H16B H 0.348(4) -0.1380(14) 0.6486(14) 0.031(8) Uiso 1 1 d . . . H17A H 0.265(5) -0.111(2) 0.7455(15) 0.042(11) Uiso 1 1 d . . . H17B H 0.372(5) -0.0558(18) 0.7505(16) 0.045(10) Uiso 1 1 d . . . H17C H 0.228(4) -0.0517(17) 0.7090(15) 0.044(10) Uiso 1 1 d . . . H18A H 0.690(3) -0.0489(14) 0.5841(12) 0.021(7) Uiso 1 1 d . . . H18B H 0.716(4) -0.0942(14) 0.6374(13) 0.024(8) Uiso 1 1 d . . . H19A H 0.586(4) -0.1798(15) 0.5893(14) 0.030(8) Uiso 1 1 d . . . H19B H 0.714(4) -0.1511(16) 0.5440(15) 0.040(9) Uiso 1 1 d . . . H19C H 0.529(5) -0.1335(16) 0.5369(18) 0.042(11) Uiso 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 C1 0.0159(13) 0.0166(12) 0.0158(12) -0.0017(10) -0.0026(10) 0.0037(10) C2 0.0183(13) 0.0213(14) 0.0170(13) -0.0029(10) 0.0037(11) -0.0008(11) C3 0.0146(13) 0.0244(14) 0.0214(14) -0.0043(11) 0.0004(11) -0.0056(11) C4 0.0150(13) 0.0180(12) 0.0161(12) 0.0005(10) -0.0016(10) 0.0016(10) C5 0.0183(13) 0.0174(13) 0.0170(12) 0.0013(10) 0.0014(11) 0.0006(11) C6 0.0141(13) 0.0170(12) 0.0204(13) 0.0008(10) 0.0006(10) -0.0021(11) C7 0.0145(13) 0.0180(12) 0.0167(12) -0.0002(10) -0.0018(10) 0.0037(10) C8 0.0164(13) 0.0210(13) 0.0150(13) 0.0009(11) 0.0016(10) -0.0008(11) C9 0.0217(14) 0.0155(13) 0.0187(14) 0.0021(10) -0.0027(11) -0.0016(11) C10 0.0190(13) 0.0157(12) 0.0160(12) -0.0002(10) -0.0031(10) 0.0029(11) C11 0.0185(14) 0.0176(12) 0.0160(12) 0.0034(10) 0.0018(11) 0.0008(11) C12 0.0157(13) 0.0160(13) 0.0190(13) 0.0011(10) -0.0008(10) -0.0004(11) C13 0.0207(15) 0.0251(14) 0.0172(13) -0.0013(11) 0.0001(11) 0.0020(12) C14 0.0250(15) 0.0269(15) 0.0157(13) -0.0026(11) -0.0021(11) 0.0046(12) C15 0.0194(15) 0.0269(14) 0.0208(14) -0.0059(12) -0.0022(12) 0.0011(12) C16 0.0246(15) 0.0264(15) 0.0262(15) -0.0029(12) 0.0009(13) -0.0024(13) C17 0.0372(19) 0.0380(18) 0.0279(16) -0.0046(15) 0.0071(15) -0.0039(16) C18 0.0179(14) 0.0251(15) 0.0300(15) -0.0034(12) -0.0001(12) 0.0012(12) C19 0.0247(17) 0.0258(16) 0.0330(16) -0.0058(13) 0.0056(14) -0.0007(13) N1 0.0204(13) 0.0172(12) 0.0160(11) -0.0032(9) -0.0007(9) -0.0009(10) N2 0.0187(11) 0.0193(11) 0.0229(12) -0.0031(9) 0.0001(9) 0.0007(9) S1 0.0118(3) 0.0186(3) 0.0155(3) -0.0023(2) -0.0005(2) -0.0005(2) S2 0.0203(3) 0.0169(3) 0.0130(3) -0.0009(2) -0.0005(2) -0.0016(3) Cd1 0.01443(13) 0.01773(12) 0.01285(12) -0.00117(7) -0.00007(7) -0.00035(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C6 1.391(3) . ? C1 C2 1.394(4) . ? C1 S1 1.779(2) . ? C2 C3 1.384(4) . ? C2 H2 0.93(3) . ? C3 C4 1.404(4) . ? C3 H3 0.98(3) . ? C4 C5 1.401(4) . ? C4 C7 1.482(3) . ? C5 C6 1.378(4) . ? C5 H5 0.96(3) . ? C6 H6 0.95(3) . ? C7 C12 1.399(4) . ? C7 C8 1.403(4) . ? C8 C9 1.380(4) . ? C8 H8 0.95(3) . ? C9 C10 1.398(4) . ? C9 H9 0.99(3) . ? C10 C11 1.401(4) . ? C10 S2 1.772(3) . ? C11 C12 1.386(4) . ? C11 H11 0.92(3) . ? C12 H12 0.91(3) . ? C13 N1 1.487(3) . ? C13 C14 1.518(4) . ? C13 H3A 0.96(3) . ? C13 H13B 1.00(3) . ? C14 C15 1.530(4) . ? C14 H14A 0.99(3) . ? C14 H14B 1.01(3) . ? C15 N2 1.472(3) . ? C15 H15A 0.97(3) . ? C15 H15B 0.97(3) . ? C16 N2 1.469(4) . ? C16 C17 1.519(4) . ? C16 H16A 0.95(3) . ? C16 H16B 1.00(3) . ? C17 H17A 0.90(4) . ? C17 H17B 0.94(4) . ? C17 H17C 1.00(4) . ? C18 N2 1.478(3) . ? C18 C19 1.527(4) . ? C18 H18A 1.00(3) . ? C18 H18B 0.94(3) . ? C19 H19A 0.97(3) . ? C19 H19B 0.99(4) . ? C19 H19C 0.99(4) . ? N1 Cd1 2.248(2) . ? N1 H1A 0.88(3) . ? N1 H1B 0.87(3) . ? S1 Cd1 2.5620(6) . ? S1 Cd1 2.5718(6) 6_657 ? S2 Cd1 2.4795(6) 3_557 ? Cd1 S2 2.4796(6) 3_457 ? Cd1 S1 2.5719(6) 6_557 ? 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 C6 C1 C2 118.3(2) . . ? C6 C1 S1 122.53(19) . . ? C2 C1 S1 119.12(19) . . ? C3 C2 C1 120.3(2) . . ? C3 C2 H2 120.5(18) . . ? C1 C2 H2 119.1(18) . . ? C2 C3 C4 121.9(2) . . ? C2 C3 H3 121.0(19) . . ? C4 C3 H3 117.1(19) . . ? C5 C4 C3 116.8(2) . . ? C5 C4 C7 121.9(2) . . ? C3 C4 C7 121.3(2) . . ? C6 C5 C4 121.4(2) . . ? C6 C5 H5 116.8(17) . . ? C4 C5 H5 121.8(17) . . ? C5 C6 C1 121.2(2) . . ? C5 C6 H6 118.0(16) . . ? C1 C6 H6 120.8(16) . . ? C12 C7 C8 116.8(2) . . ? C12 C7 C4 121.8(2) . . ? C8 C7 C4 121.4(2) . . ? C9 C8 C7 121.7(2) . . ? C9 C8 H8 117.4(18) . . ? C7 C8 H8 121.0(18) . . ? C8 C9 C10 121.5(2) . . ? C8 C9 H9 117.3(16) . . ? C10 C9 H9 121.2(16) . . ? C9 C10 C11 117.2(2) . . ? C9 C10 S2 118.8(2) . . ? C11 C10 S2 124.0(2) . . ? C12 C11 C10 121.3(2) . . ? C12 C11 H11 116.1(16) . . ? C10 C11 H11 122.6(16) . . ? C11 C12 C7 121.6(2) . . ? C11 C12 H12 117.1(17) . . ? C7 C12 H12 121.4(17) . . ? N1 C13 C14 113.6(2) . . ? N1 C13 H3A 106.5(17) . . ? C14 C13 H3A 108.1(17) . . ? N1 C13 H13B 108(2) . . ? C14 C13 H13B 113(2) . . ? H3A C13 H13B 108(2) . . ? C13 C14 C15 113.4(2) . . ? C13 C14 H14A 109.9(16) . . ? C15 C14 H14A 106.7(16) . . ? C13 C14 H14B 111.4(16) . . ? C15 C14 H14B 110.7(16) . . ? H14A C14 H14B 104(2) . . ? N2 C15 C14 112.8(2) . . ? N2 C15 H15A 106.4(16) . . ? C14 C15 H15A 108.3(16) . . ? N2 C15 H15B 109.6(16) . . ? C14 C15 H15B 111.3(16) . . ? H15A C15 H15B 108(2) . . ? N2 C16 C17 112.5(3) . . ? N2 C16 H16A 106(2) . . ? C17 C16 H16A 112(2) . . ? N2 C16 H16B 112.3(18) . . ? C17 C16 H16B 110.4(18) . . ? H16A C16 H16B 103(3) . . ? C16 C17 H17A 112(2) . . ? C16 C17 H17B 115(2) . . ? H17A C17 H17B 106(3) . . ? C16 C17 H17C 113(2) . . ? H17A C17 H17C 107(3) . . ? H17B C17 H17C 103(3) . . ? N2 C18 C19 115.8(2) . . ? N2 C18 H18A 107.1(16) . . ? C19 C18 H18A 110.8(16) . . ? N2 C18 H18B 105.6(18) . . ? C19 C18 H18B 110.9(18) . . ? H18A C18 H18B 106(2) . . ? C18 C19 H19A 112.5(19) . . ? C18 C19 H19B 110(2) . . ? H19A C19 H19B 108(3) . . ? C18 C19 H19C 111(2) . . ? H19A C19 H19C 110(3) . . ? H19B C19 H19C 105(3) . . ? C13 N1 Cd1 116.97(16) . . ? C13 N1 H1A 108.8(19) . . ? Cd1 N1 H1A 108(2) . . ? C13 N1 H1B 110(2) . . ? Cd1 N1 H1B 107(2) . . ? H1A N1 H1B 105(3) . . ? C16 N2 C15 112.4(2) . . ? C16 N2 C18 111.8(2) . . ? C15 N2 C18 111.5(2) . . ? C1 S1 Cd1 108.79(9) . . ? C1 S1 Cd1 103.97(8) . 6_657 ? Cd1 S1 Cd1 107.67(2) . 6_657 ? C10 S2 Cd1 107.28(9) . 3_557 ? N1 Cd1 S2 107.92(6) . 3_457 ? N1 Cd1 S1 100.17(7) . . ? S2 Cd1 S1 125.92(2) 3_457 . ? N1 Cd1 S1 107.48(6) . 6_557 ? S2 Cd1 S1 107.25(2) 3_457 6_557 ? S1 Cd1 S1 106.85(2) . 6_557 ? 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 H1A N2 0.88(3) 2.18(3) 2.895(3) 138(3) . N1 H1B S2 0.87(3) 2.64(3) 3.464(2) 158(3) 8_565 # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _chemical_name_common 'N,N-diethyl-1,3-propanediamine biphenyldithiolate cadmium(ii)'