# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef 'C2CE25082A-ccdc-860863-860865-cif.txt' _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email jianzhou888888@163.com _publ_contact_author_name 'Jian Zhou' loop_ _publ_author_name 'Xing Liu' 'Jian Zhou' data_1 _database_code_depnum_ccdc_archive 'CCDC 860863' #TrackingRef 'ce-art-01-2012-025082-File005-v1-0.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C6 H20 N4), Ge2 S6' _chemical_formula_sum 'C12 H40 Ge2 N8 S6 ' _chemical_formula_weight 634.16 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.264(9) _cell_length_b 7.313(3) _cell_length_c 16.584(6) _cell_angle_alpha 90.00 _cell_angle_beta 122.616(4) _cell_angle_gamma 90.00 _cell_volume 2580.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 25.10 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 2.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2201 _exptl_absorpt_correction_T_max 0.3255 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6151 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0896 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.10 _reflns_number_total 2261 _reflns_number_gt 2078 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+6.4132P] 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 2261 _refine_ls_number_parameters 159 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.035 _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 Ge1 Ge 0.546039(18) 0.40952(4) 0.47821(3) 0.02105(17) Uani 1 1 d . . . S1 S 0.51719(5) 0.17937(11) 0.38135(7) 0.0281(3) Uani 1 1 d . . . S2 S 0.47598(5) 0.64361(11) 0.40815(7) 0.0248(3) Uani 1 1 d . . . S3 S 0.64073(5) 0.50241(12) 0.53777(8) 0.0330(3) Uani 1 1 d . . . N1 N 0.9178(2) 0.6792(5) 0.6836(3) 0.0367(9) Uani 1 1 d . . . N2 N 0.90037(19) 0.0681(4) 0.6959(3) 0.0321(8) Uani 1 1 d D . . N3 N 0.83082(17) 0.4023(3) 0.7062(3) 0.0262(8) Uani 1 1 d . . . N4 N 0.90666(19) 0.4051(4) 0.9261(3) 0.0299(8) Uani 1 1 d . . . C1 C 0.8555(2) 0.6099(5) 0.6109(3) 0.0355(11) Uani 1 1 d . . . H1A H 0.8598 0.4967 0.5846 0.043 Uiso 1 1 calc R . . H1B H 0.8344 0.6979 0.5592 0.043 Uiso 1 1 calc R . . C2 C 0.8160(2) 0.5761(5) 0.6533(4) 0.0361(11) Uani 1 1 d . . . H2C H 0.8225 0.6760 0.6962 0.043 Uiso 1 1 calc R . . H2D H 0.7720 0.5759 0.6020 0.043 Uiso 1 1 calc R . . C3 C 0.8373(2) 0.0698(5) 0.6813(4) 0.0336(10) Uani 1 1 d . . . H3A H 0.8414 0.0498 0.7422 0.040 Uiso 1 1 calc R . . H3B H 0.8126 -0.0297 0.6389 0.040 Uiso 1 1 calc R . . C4 C 0.8030(2) 0.2489(5) 0.6388(3) 0.0324(9) Uani 1 1 d . . . H4D H 0.8038 0.2767 0.5822 0.039 Uiso 1 1 calc R . . H4E H 0.7595 0.2351 0.6190 0.039 Uiso 1 1 calc R . . C5 C 0.8478(2) 0.5059(5) 0.8613(3) 0.0332(10) Uani 1 1 d . . . H5A H 0.8579 0.6250 0.8474 0.040 Uiso 1 1 calc R . . H5B H 0.8252 0.5245 0.8929 0.040 Uiso 1 1 calc R . . C6 C 0.8064(2) 0.4032(5) 0.7687(3) 0.0302(9) Uani 1 1 d . . . H6A H 0.8019 0.2779 0.7834 0.036 Uiso 1 1 calc R . . H6B H 0.7649 0.4584 0.7346 0.036 Uiso 1 1 calc R . . H4C H 0.930(2) 0.463(6) 0.981(4) 0.028(11) Uiso 1 1 d . . . H4B H 0.928(2) 0.391(5) 0.900(4) 0.038(12) Uiso 1 1 d . . . H2G H 0.899(3) 0.103(6) 0.643(3) 0.052(15) Uiso 1 1 d D . . H4A H 0.895(2) 0.297(6) 0.936(3) 0.040(12) Uiso 1 1 d . . . H2F H 0.925(2) 0.148(5) 0.743(3) 0.045(13) Uiso 1 1 d D . . H2E H 0.916(2) -0.048(4) 0.712(4) 0.056(15) Uiso 1 1 d D . . H1J H 0.932(3) 0.604(8) 0.726(5) 0.07(2) Uiso 1 1 d . . . H1G H 0.938(3) 0.684(7) 0.663(4) 0.059(17) 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 Ge1 0.0233(3) 0.0202(2) 0.0222(3) 0.00063(13) 0.0140(3) 0.00108(13) S1 0.0353(7) 0.0244(4) 0.0268(6) -0.0041(4) 0.0182(6) 0.0009(4) S2 0.0324(6) 0.0231(4) 0.0222(6) 0.0046(3) 0.0169(5) 0.0045(4) S3 0.0246(6) 0.0349(5) 0.0404(7) 0.0004(4) 0.0180(6) -0.0021(4) N1 0.037(3) 0.0382(19) 0.038(3) -0.0027(17) 0.022(2) 0.0001(17) N2 0.039(3) 0.0307(17) 0.030(2) 0.0020(15) 0.021(2) 0.0010(15) N3 0.028(2) 0.0205(14) 0.028(2) 0.0006(12) 0.0135(19) 0.0003(12) N4 0.030(2) 0.0291(17) 0.027(2) -0.0027(14) 0.013(2) -0.0006(14) C1 0.047(3) 0.0304(18) 0.033(3) 0.0031(16) 0.024(3) 0.0002(18) C2 0.042(3) 0.0242(18) 0.048(3) 0.0077(17) 0.028(3) 0.0069(16) C3 0.036(3) 0.0239(17) 0.043(3) -0.0025(16) 0.022(3) -0.0024(16) C4 0.035(3) 0.0264(17) 0.033(3) -0.0022(16) 0.016(2) -0.0022(16) C5 0.035(3) 0.0292(18) 0.034(3) 0.0015(16) 0.017(2) 0.0108(17) C6 0.030(3) 0.0303(18) 0.030(3) 0.0020(15) 0.016(2) -0.0003(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 S3 2.1477(13) . ? Ge1 S1 2.1638(11) . ? Ge1 S2 2.2678(10) 5_666 ? Ge1 S2 2.2796(11) . ? S2 Ge1 2.2678(10) 5_666 ? N1 C1 1.464(6) . ? N1 H1J 0.81(7) . ? N1 H1G 0.76(6) . ? N2 C3 1.478(6) . ? N2 H2G 0.889(19) . ? N2 H2F 0.90(2) . ? N2 H2E 0.911(19) . ? N3 C6 1.465(5) . ? N3 C4 1.469(5) . ? N3 C2 1.474(4) . ? N4 C5 1.479(6) . ? N4 H4C 0.89(5) . ? N4 H4B 0.87(5) . ? N4 H4A 0.90(5) . ? C1 C2 1.517(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.517(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4D 0.9700 . ? C4 H4E 0.9700 . ? C5 C6 1.512(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? 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 S3 Ge1 S1 115.69(4) . . ? S3 Ge1 S2 112.54(5) . 5_666 ? S1 Ge1 S2 110.38(4) . 5_666 ? S3 Ge1 S2 111.30(4) . . ? S1 Ge1 S2 110.33(5) . . ? S2 Ge1 S2 94.67(4) 5_666 . ? Ge1 S2 Ge1 85.33(4) 5_666 . ? C1 N1 H1J 105(5) . . ? C1 N1 H1G 110(4) . . ? H1J N1 H1G 110(6) . . ? C3 N2 H2G 112(4) . . ? C3 N2 H2F 108(3) . . ? H2G N2 H2F 108(4) . . ? C3 N2 H2E 108(3) . . ? H2G N2 H2E 110(4) . . ? H2F N2 H2E 112(5) . . ? C6 N3 C4 109.4(3) . . ? C6 N3 C2 110.5(3) . . ? C4 N3 C2 109.9(3) . . ? C5 N4 H4C 111(3) . . ? C5 N4 H4B 111(3) . . ? H4C N4 H4B 109(4) . . ? C5 N4 H4A 105(3) . . ? H4C N4 H4A 110(4) . . ? H4B N4 H4A 111(4) . . ? N1 C1 C2 111.0(4) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N3 C2 C1 113.4(3) . . ? N3 C2 H2C 108.9 . . ? C1 C2 H2C 108.9 . . ? N3 C2 H2D 108.9 . . ? C1 C2 H2D 108.9 . . ? H2C C2 H2D 107.7 . . ? N2 C3 C4 112.2(3) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C3 112.8(4) . . ? N3 C4 H4D 109.0 . . ? C3 C4 H4D 109.0 . . ? N3 C4 H4E 109.0 . . ? C3 C4 H4E 109.0 . . ? H4D C4 H4E 107.8 . . ? N4 C5 C6 111.4(3) . . ? N4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? N3 C6 C5 113.3(3) . . ? N3 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? N3 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S3 Ge1 S2 Ge1 -116.40(4) . . . 5_666 ? S1 Ge1 S2 Ge1 113.76(4) . . . 5_666 ? S2 Ge1 S2 Ge1 0.0 5_666 . . 5_666 ? C6 N3 C2 C1 162.6(4) . . . . ? C4 N3 C2 C1 -76.6(5) . . . . ? N1 C1 C2 N3 -79.9(4) . . . . ? C6 N3 C4 C3 -83.3(4) . . . . ? C2 N3 C4 C3 155.2(3) . . . . ? N2 C3 C4 N3 -69.8(4) . . . . ? C4 N3 C6 C5 158.7(3) . . . . ? C2 N3 C6 C5 -80.2(4) . . . . ? N4 C5 C6 N3 -71.3(4) . . . . ? 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 H4C S1 0.89(5) 2.49(5) 3.361(4) 169(4) 4_656 N4 H4B S1 0.87(5) 2.48(5) 3.311(4) 160(4) 8_556 N2 H2G S3 0.889(19) 2.71(3) 3.467(4) 143(4) 7_656 N2 H2G S1 0.889(19) 2.85(4) 3.502(3) 131(4) 7_656 N4 H4A S3 0.90(5) 2.46(5) 3.352(4) 179(4) 4_646 N2 H2F S1 0.90(2) 2.56(2) 3.434(4) 165(4) 8_556 N2 H2E N1 0.911(19) 2.06(3) 2.902(5) 153(5) 1_545 N2 H2E S2 0.911(19) 2.83(5) 3.345(4) 117(4) 8_556 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.553 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.148 # Attachment 'ce-art-01-2012-025082-File006-v1-0.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 860864' #TrackingRef 'ce-art-01-2012-025082-File006-v1-0.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H39 Eu N9, 0.5(Ge2 S6), Cl ' _chemical_formula_sum 'C12 H39 Cl Eu Ge N9 S3 ' _chemical_formula_weight 665.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 11.567(5) _cell_length_b 14.633(6) _cell_length_c 14.465(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.434(4) _cell_angle_gamma 90.00 _cell_volume 2432.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 25.09 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 4.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6129 _exptl_absorpt_correction_T_max 0.7587 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12834 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.09 _reflns_number_total 4308 _reflns_number_gt 3984 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+2.8141P] 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 4308 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 1.001110(13) 0.241621(11) 0.690289(12) 0.02206(8) Uani 1 1 d . . . N1 N 1.0579(3) 0.4142(2) 0.7049(2) 0.0361(7) Uani 1 1 d . . . H1A H 1.0685 0.4296 0.7655 0.043 Uiso 1 1 calc R . . H1B H 1.1258 0.4228 0.6812 0.043 Uiso 1 1 calc R . . N2 N 0.8305(3) 0.3596(2) 0.6982(3) 0.0469(9) Uani 1 1 d . . . H2C H 0.8276 0.3632 0.7607 0.056 Uiso 1 1 calc R . . N3 N 0.7909(2) 0.1720(2) 0.6755(2) 0.0365(8) Uani 1 1 d . . . H3A H 0.7707 0.1564 0.6157 0.044 Uiso 1 1 calc R . . H3B H 0.7928 0.1204 0.7095 0.044 Uiso 1 1 calc R . . N4 N 0.9241(3) 0.2745(2) 0.5176(2) 0.0391(8) Uani 1 1 d . . . H4A H 0.8695 0.2325 0.4990 0.047 Uiso 1 1 calc R . . H4B H 0.8889 0.3295 0.5148 0.047 Uiso 1 1 calc R . . N5 N 1.1644(3) 0.2567(2) 0.5792(2) 0.0309(7) Uani 1 1 d . . . H5C H 1.1751 0.1992 0.5578 0.037 Uiso 1 1 calc R . . N6 N 1.2147(3) 0.2370(2) 0.7731(2) 0.0300(7) Uani 1 1 d . . . H6A H 1.2274 0.2885 0.8068 0.036 Uiso 1 1 calc R . . H6B H 1.2206 0.1897 0.8132 0.036 Uiso 1 1 calc R . . N7 N 1.0118(3) 0.0811(2) 0.6040(2) 0.0394(8) Uani 1 1 d . . . H7A H 0.9413 0.0683 0.5738 0.047 Uiso 1 1 calc R . . H7B H 1.0623 0.0856 0.5613 0.047 Uiso 1 1 calc R . . N8 N 1.0141(2) 0.0996(2) 0.7991(2) 0.0321(7) Uani 1 1 d . . . H8C H 1.0911 0.0957 0.8202 0.039 Uiso 1 1 calc R . . N9 N 0.9864(3) 0.2776(2) 0.8659(2) 0.0379(8) Uani 1 1 d . . . H9A H 1.0392 0.3209 0.8844 0.046 Uiso 1 1 calc R . . H9B H 0.9155 0.3012 0.8709 0.046 Uiso 1 1 calc R . . C1 C 0.9686(4) 0.4748(3) 0.6560(4) 0.0519(12) Uani 1 1 d . . . H1C H 0.9867 0.5375 0.6738 0.062 Uiso 1 1 calc R . . H1D H 0.9723 0.4697 0.5895 0.062 Uiso 1 1 calc R . . C2 C 0.8497(4) 0.4543(3) 0.6755(4) 0.0510(11) Uani 1 1 d . . . H2A H 0.8315 0.4921 0.7270 0.061 Uiso 1 1 calc R . . H2B H 0.7963 0.4708 0.6216 0.061 Uiso 1 1 calc R . . C3 C 0.7138(3) 0.3250(3) 0.6667(4) 0.0556(14) Uani 1 1 d . . . H3C H 0.7026 0.3228 0.5993 0.067 Uiso 1 1 calc R . . H3D H 0.6557 0.3657 0.6875 0.067 Uiso 1 1 calc R . . C4 C 0.6998(4) 0.2320(3) 0.7052(4) 0.0621(16) Uani 1 1 d . . . H4C H 0.7063 0.2346 0.7726 0.075 Uiso 1 1 calc R . . H4D H 0.6236 0.2080 0.6829 0.075 Uiso 1 1 calc R . . C5 C 1.0119(4) 0.2742(3) 0.4509(3) 0.0404(10) Uani 1 1 d . . . H5A H 0.9846 0.3113 0.3973 0.049 Uiso 1 1 calc R . . H5B H 1.0228 0.2123 0.4295 0.049 Uiso 1 1 calc R . . C6 C 1.1263(3) 0.3113(3) 0.4958(3) 0.0365(9) Uani 1 1 d . . . H6C H 1.1842 0.3083 0.4523 0.044 Uiso 1 1 calc R . . H6D H 1.1172 0.3748 0.5130 0.044 Uiso 1 1 calc R . . C7 C 1.2790(3) 0.2849(3) 0.6260(3) 0.0403(10) Uani 1 1 d . . . H7C H 1.2770 0.3491 0.6427 0.048 Uiso 1 1 calc R . . H7D H 1.3382 0.2768 0.5841 0.048 Uiso 1 1 calc R . . C8 C 1.3079(3) 0.2283(3) 0.7113(3) 0.0420(10) Uani 1 1 d . . . H8A H 1.3159 0.1648 0.6939 0.050 Uiso 1 1 calc R . . H8B H 1.3813 0.2483 0.7439 0.050 Uiso 1 1 calc R . . C9 C 1.0479(4) 0.0051(3) 0.6676(3) 0.0470(11) Uani 1 1 d . . . H9C H 1.1315 0.0075 0.6844 0.056 Uiso 1 1 calc R . . H9D H 1.0293 -0.0526 0.6365 0.056 Uiso 1 1 calc R . . C10 C 0.9875(4) 0.0109(3) 0.7536(3) 0.0440(10) Uani 1 1 d . . . H10A H 0.9041 0.0049 0.7374 0.053 Uiso 1 1 calc R . . H10B H 1.0135 -0.0384 0.7957 0.053 Uiso 1 1 calc R . . C11 C 0.9570(4) 0.1136(3) 0.8843(3) 0.0479(11) Uani 1 1 d . . . H11A H 0.9721 0.0620 0.9260 0.057 Uiso 1 1 calc R . . H11B H 0.8735 0.1192 0.8686 0.057 Uiso 1 1 calc R . . C12 C 1.0048(4) 0.1991(4) 0.9302(3) 0.0493(11) Uani 1 1 d . . . H12A H 0.9667 0.2108 0.9855 0.059 Uiso 1 1 calc R . . H12B H 1.0874 0.1916 0.9492 0.059 Uiso 1 1 calc R . . Ge1 Ge 0.36302(3) -0.00032(2) 0.49327(2) 0.02204(10) Uani 1 1 d . . . S1 S 0.24708(7) 0.09886(7) 0.42177(7) 0.0371(2) Uani 1 1 d . . . S2 S 0.26845(8) -0.10689(8) 0.55576(7) 0.0381(2) Uani 1 1 d . . . S3 S 0.50509(7) 0.05900(7) 0.59749(7) 0.0365(2) Uani 1 1 d . . . Cl1 Cl 0.26769(9) 0.04965(8) 0.91360(8) 0.0476(3) 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 Eu1 0.01837(10) 0.02287(12) 0.02534(13) -0.00387(6) 0.00415(8) 0.00043(6) N1 0.0418(17) 0.0316(18) 0.0342(18) -0.0033(14) 0.0011(14) -0.0016(14) N2 0.0313(16) 0.040(2) 0.069(3) -0.0084(18) -0.0001(16) 0.0057(15) N3 0.0293(15) 0.039(2) 0.042(2) -0.0075(15) 0.0063(14) -0.0029(14) N4 0.0333(17) 0.0378(19) 0.044(2) 0.0061(16) -0.0068(15) -0.0038(14) N5 0.0302(16) 0.0364(19) 0.0271(18) 0.0000(12) 0.0081(14) -0.0008(12) N6 0.0268(15) 0.0320(18) 0.0319(19) 0.0001(13) 0.0069(13) -0.0020(12) N7 0.0390(17) 0.038(2) 0.043(2) -0.0126(16) 0.0123(15) -0.0049(15) N8 0.0283(14) 0.0346(19) 0.0337(18) 0.0033(13) 0.0040(13) -0.0067(13) N9 0.0277(16) 0.047(2) 0.041(2) -0.0149(17) 0.0099(14) 0.0000(14) C1 0.057(3) 0.035(3) 0.065(3) 0.013(2) 0.017(2) 0.008(2) C2 0.053(2) 0.036(3) 0.063(3) 0.000(2) 0.000(2) 0.013(2) C3 0.029(2) 0.054(3) 0.081(4) -0.028(3) -0.010(2) 0.0145(19) C4 0.032(2) 0.062(3) 0.095(4) -0.038(3) 0.019(2) -0.012(2) C5 0.055(2) 0.036(2) 0.028(2) 0.0007(17) -0.0042(19) -0.0006(19) C6 0.046(2) 0.039(2) 0.026(2) 0.0027(16) 0.0077(17) -0.0052(17) C7 0.0241(18) 0.066(3) 0.033(2) 0.001(2) 0.0089(15) -0.0073(18) C8 0.0222(18) 0.069(3) 0.036(2) -0.006(2) 0.0045(16) 0.0071(18) C9 0.039(2) 0.033(2) 0.069(3) -0.015(2) 0.006(2) 0.0025(18) C10 0.043(2) 0.032(2) 0.056(3) 0.0077(19) -0.002(2) -0.0064(18) C11 0.044(2) 0.057(3) 0.045(3) 0.010(2) 0.0160(19) -0.011(2) C12 0.047(2) 0.074(3) 0.030(2) -0.005(2) 0.0166(19) -0.008(2) Ge1 0.01735(17) 0.0241(2) 0.0250(2) -0.00108(14) 0.00396(14) -0.00062(13) S1 0.0284(4) 0.0369(6) 0.0455(6) 0.0095(4) 0.0023(4) 0.0067(4) S2 0.0314(4) 0.0426(6) 0.0402(6) 0.0113(4) 0.0042(4) -0.0108(4) S3 0.0227(4) 0.0501(6) 0.0374(5) -0.0209(5) 0.0059(4) -0.0028(4) Cl1 0.0432(5) 0.0397(6) 0.0575(7) -0.0012(5) -0.0054(5) 0.0085(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 Eu1 N8 2.601(3) . ? Eu1 N4 2.601(3) . ? Eu1 N1 2.612(3) . ? Eu1 N9 2.618(3) . ? Eu1 N5 2.623(3) . ? Eu1 N6 2.623(3) . ? Eu1 N3 2.623(3) . ? Eu1 N2 2.633(3) . ? Eu1 N7 2.669(3) . ? N1 C1 1.480(5) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.447(6) . ? N2 C3 1.466(5) . ? N2 H2C 0.9100 . ? N3 C4 1.472(5) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C5 1.477(6) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C6 1.472(5) . ? N5 C7 1.478(5) . ? N5 H5C 0.9100 . ? N6 C8 1.481(5) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 C9 1.474(6) . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? N8 C10 1.473(5) . ? N8 C11 1.477(5) . ? N8 H8C 0.9100 . ? N9 C12 1.479(6) . ? N9 H9A 0.9000 . ? N9 H9B 0.9000 . ? C1 C2 1.466(6) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.486(7) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 C6 1.508(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 C8 1.493(6) . ? C7 H7C 0.9700 . ? C7 H7D 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.496(7) . ? C9 H9C 0.9700 . ? C9 H9D 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.493(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? Ge1 S1 2.1595(11) . ? Ge1 S2 2.1604(11) . ? Ge1 S3 2.2740(11) . ? Ge1 S3 2.2884(11) 3_656 ? S3 Ge1 2.2884(11) 3_656 ? 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 N8 Eu1 N4 136.00(10) . . ? N8 Eu1 N1 136.60(10) . . ? N4 Eu1 N1 87.40(11) . . ? N8 Eu1 N9 65.12(11) . . ? N4 Eu1 N9 147.34(11) . . ? N1 Eu1 N9 76.72(11) . . ? N8 Eu1 N5 116.20(10) . . ? N4 Eu1 N5 65.71(11) . . ? N1 Eu1 N5 77.06(10) . . ? N9 Eu1 N5 135.00(10) . . ? N8 Eu1 N6 73.47(9) . . ? N4 Eu1 N6 130.32(10) . . ? N1 Eu1 N6 76.84(10) . . ? N9 Eu1 N6 73.88(10) . . ? N5 Eu1 N6 64.92(10) . . ? N8 Eu1 N3 74.31(10) . . ? N4 Eu1 N3 77.22(11) . . ? N1 Eu1 N3 127.19(10) . . ? N9 Eu1 N3 89.82(10) . . ? N5 Eu1 N3 135.02(10) . . ? N6 Eu1 N3 147.62(10) . . ? N8 Eu1 N2 119.36(11) . . ? N4 Eu1 N2 75.08(12) . . ? N1 Eu1 N2 62.98(11) . . ? N9 Eu1 N2 72.28(12) . . ? N5 Eu1 N2 124.44(11) . . ? N6 Eu1 N2 131.98(11) . . ? N3 Eu1 N2 64.27(11) . . ? N8 Eu1 N7 64.99(11) . . ? N4 Eu1 N7 75.10(11) . . ? N1 Eu1 N7 149.80(10) . . ? N9 Eu1 N7 129.94(11) . . ? N5 Eu1 N7 73.36(10) . . ? N6 Eu1 N7 95.77(10) . . ? N3 Eu1 N7 73.21(10) . . ? N2 Eu1 N7 132.15(10) . . ? C1 N1 Eu1 112.6(3) . . ? C1 N1 H1A 109.1 . . ? Eu1 N1 H1A 109.1 . . ? C1 N1 H1B 109.1 . . ? Eu1 N1 H1B 109.1 . . ? H1A N1 H1B 107.8 . . ? C2 N2 C3 114.8(3) . . ? C2 N2 Eu1 118.9(3) . . ? C3 N2 Eu1 115.4(3) . . ? C2 N2 H2C 101.1 . . ? C3 N2 H2C 101.1 . . ? Eu1 N2 H2C 101.1 . . ? C4 N3 Eu1 115.6(2) . . ? C4 N3 H3A 108.4 . . ? Eu1 N3 H3A 108.4 . . ? C4 N3 H3B 108.4 . . ? Eu1 N3 H3B 108.4 . . ? H3A N3 H3B 107.4 . . ? C5 N4 Eu1 116.1(2) . . ? C5 N4 H4A 108.3 . . ? Eu1 N4 H4A 108.3 . . ? C5 N4 H4B 108.3 . . ? Eu1 N4 H4B 108.3 . . ? H4A N4 H4B 107.4 . . ? C6 N5 C7 113.2(3) . . ? C6 N5 Eu1 112.2(2) . . ? C7 N5 Eu1 114.4(2) . . ? C6 N5 H5C 105.3 . . ? C7 N5 H5C 105.3 . . ? Eu1 N5 H5C 105.3 . . ? C8 N6 Eu1 116.0(2) . . ? C8 N6 H6A 108.3 . . ? Eu1 N6 H6A 108.3 . . ? C8 N6 H6B 108.3 . . ? Eu1 N6 H6B 108.3 . . ? H6A N6 H6B 107.4 . . ? C9 N7 Eu1 113.4(2) . . ? C9 N7 H7A 108.9 . . ? Eu1 N7 H7A 108.9 . . ? C9 N7 H7B 108.9 . . ? Eu1 N7 H7B 108.9 . . ? H7A N7 H7B 107.7 . . ? C10 N8 C11 113.9(3) . . ? C10 N8 Eu1 116.0(2) . . ? C11 N8 Eu1 113.1(3) . . ? C10 N8 H8C 104.0 . . ? C11 N8 H8C 104.0 . . ? Eu1 N8 H8C 104.0 . . ? C12 N9 Eu1 115.7(3) . . ? C12 N9 H9A 108.3 . . ? Eu1 N9 H9A 108.3 . . ? C12 N9 H9B 108.3 . . ? Eu1 N9 H9B 108.3 . . ? H9A N9 H9B 107.4 . . ? C2 C1 N1 113.9(4) . . ? C2 C1 H1C 108.8 . . ? N1 C1 H1C 108.8 . . ? C2 C1 H1D 108.8 . . ? N1 C1 H1D 108.8 . . ? H1C C1 H1D 107.7 . . ? N2 C2 C1 114.2(4) . . ? N2 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? N2 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N2 C3 C4 109.6(4) . . ? N2 C3 H3C 109.8 . . ? C4 C3 H3C 109.8 . . ? N2 C3 H3D 109.8 . . ? C4 C3 H3D 109.8 . . ? H3C C3 H3D 108.2 . . ? N3 C4 C3 109.0(4) . . ? N3 C4 H4C 109.9 . . ? C3 C4 H4C 109.9 . . ? N3 C4 H4D 109.9 . . ? C3 C4 H4D 109.9 . . ? H4C C4 H4D 108.3 . . ? N4 C5 C6 110.6(3) . . ? N4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? N5 C6 C5 109.0(3) . . ? N5 C6 H6C 109.9 . . ? C5 C6 H6C 109.9 . . ? N5 C6 H6D 109.9 . . ? C5 C6 H6D 109.9 . . ? H6C C6 H6D 108.3 . . ? N5 C7 C8 109.2(3) . . ? N5 C7 H7C 109.8 . . ? C8 C7 H7C 109.8 . . ? N5 C7 H7D 109.8 . . ? C8 C7 H7D 109.8 . . ? H7C C7 H7D 108.3 . . ? N6 C8 C7 109.9(3) . . ? N6 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? N6 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? N7 C9 C10 110.5(3) . . ? N7 C9 H9C 109.6 . . ? C10 C9 H9C 109.6 . . ? N7 C9 H9D 109.6 . . ? C10 C9 H9D 109.6 . . ? H9C C9 H9D 108.1 . . ? N8 C10 C9 109.1(3) . . ? N8 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? N8 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N8 C11 C12 108.0(3) . . ? N8 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? N8 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? N9 C12 C11 110.5(4) . . ? N9 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? N9 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? S1 Ge1 S2 111.66(5) . . ? S1 Ge1 S3 115.14(5) . . ? S2 Ge1 S3 111.12(5) . . ? S1 Ge1 S3 113.30(5) . 3_656 ? S2 Ge1 S3 111.75(5) . 3_656 ? S3 Ge1 S3 92.57(4) . 3_656 ? Ge1 S3 Ge1 87.43(4) . 3_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Eu1 N1 C1 -138.9(3) . . . . ? N4 Eu1 N1 C1 40.8(3) . . . . ? N9 Eu1 N1 C1 -110.4(3) . . . . ? N5 Eu1 N1 C1 106.5(3) . . . . ? N6 Eu1 N1 C1 173.3(3) . . . . ? N3 Eu1 N1 C1 -31.0(3) . . . . ? N2 Eu1 N1 C1 -33.8(3) . . . . ? N7 Eu1 N1 C1 94.6(3) . . . . ? N8 Eu1 N2 C2 150.7(3) . . . . ? N4 Eu1 N2 C2 -74.5(3) . . . . ? N1 Eu1 N2 C2 20.2(3) . . . . ? N9 Eu1 N2 C2 104.1(3) . . . . ? N5 Eu1 N2 C2 -28.9(4) . . . . ? N6 Eu1 N2 C2 56.9(4) . . . . ? N3 Eu1 N2 C2 -157.3(4) . . . . ? N7 Eu1 N2 C2 -127.6(3) . . . . ? N8 Eu1 N2 C3 -66.8(4) . . . . ? N4 Eu1 N2 C3 67.9(3) . . . . ? N1 Eu1 N2 C3 162.7(4) . . . . ? N9 Eu1 N2 C3 -113.5(4) . . . . ? N5 Eu1 N2 C3 113.6(3) . . . . ? N6 Eu1 N2 C3 -160.7(3) . . . . ? N3 Eu1 N2 C3 -14.8(3) . . . . ? N7 Eu1 N2 C3 14.8(4) . . . . ? N8 Eu1 N3 C4 118.3(4) . . . . ? N4 Eu1 N3 C4 -95.6(4) . . . . ? N1 Eu1 N3 C4 -19.0(4) . . . . ? N9 Eu1 N3 C4 54.1(4) . . . . ? N5 Eu1 N3 C4 -130.2(3) . . . . ? N6 Eu1 N3 C4 112.6(4) . . . . ? N2 Eu1 N3 C4 -16.2(4) . . . . ? N7 Eu1 N3 C4 -173.7(4) . . . . ? N8 Eu1 N4 C5 -97.3(3) . . . . ? N1 Eu1 N4 C5 83.0(3) . . . . ? N9 Eu1 N4 C5 143.2(3) . . . . ? N5 Eu1 N4 C5 6.0(3) . . . . ? N6 Eu1 N4 C5 12.7(3) . . . . ? N3 Eu1 N4 C5 -147.9(3) . . . . ? N2 Eu1 N4 C5 145.7(3) . . . . ? N7 Eu1 N4 C5 -72.2(3) . . . . ? N8 Eu1 N5 C6 155.2(2) . . . . ? N4 Eu1 N5 C6 24.1(2) . . . . ? N1 Eu1 N5 C6 -68.9(2) . . . . ? N9 Eu1 N5 C6 -124.7(2) . . . . ? N6 Eu1 N5 C6 -150.3(3) . . . . ? N3 Eu1 N5 C6 61.4(3) . . . . ? N2 Eu1 N5 C6 -25.2(3) . . . . ? N7 Eu1 N5 C6 104.9(3) . . . . ? N8 Eu1 N5 C7 -74.0(3) . . . . ? N4 Eu1 N5 C7 154.9(3) . . . . ? N1 Eu1 N5 C7 61.8(3) . . . . ? N9 Eu1 N5 C7 6.1(3) . . . . ? N6 Eu1 N5 C7 -19.5(3) . . . . ? N3 Eu1 N5 C7 -167.8(3) . . . . ? N2 Eu1 N5 C7 105.5(3) . . . . ? N7 Eu1 N5 C7 -124.3(3) . . . . ? N8 Eu1 N6 C8 119.5(3) . . . . ? N4 Eu1 N6 C8 -17.6(3) . . . . ? N1 Eu1 N6 C8 -92.5(3) . . . . ? N9 Eu1 N6 C8 -172.3(3) . . . . ? N5 Eu1 N6 C8 -10.8(3) . . . . ? N3 Eu1 N6 C8 125.2(3) . . . . ? N2 Eu1 N6 C8 -125.6(3) . . . . ? N7 Eu1 N6 C8 57.7(3) . . . . ? N8 Eu1 N7 C9 -14.3(2) . . . . ? N4 Eu1 N7 C9 -175.3(3) . . . . ? N1 Eu1 N7 C9 128.1(3) . . . . ? N9 Eu1 N7 C9 -19.4(3) . . . . ? N5 Eu1 N7 C9 116.1(3) . . . . ? N6 Eu1 N7 C9 54.4(3) . . . . ? N3 Eu1 N7 C9 -94.5(3) . . . . ? N2 Eu1 N7 C9 -122.2(3) . . . . ? N4 Eu1 N8 C10 10.5(3) . . . . ? N1 Eu1 N8 C10 -169.9(2) . . . . ? N9 Eu1 N8 C10 159.3(3) . . . . ? N5 Eu1 N8 C10 -70.9(3) . . . . ? N6 Eu1 N8 C10 -121.2(3) . . . . ? N3 Eu1 N8 C10 62.0(3) . . . . ? N2 Eu1 N8 C10 109.5(3) . . . . ? N7 Eu1 N8 C10 -16.4(2) . . . . ? N4 Eu1 N8 C11 -123.8(3) . . . . ? N1 Eu1 N8 C11 55.8(3) . . . . ? N9 Eu1 N8 C11 25.0(2) . . . . ? N5 Eu1 N8 C11 154.8(2) . . . . ? N6 Eu1 N8 C11 104.5(3) . . . . ? N3 Eu1 N8 C11 -72.3(2) . . . . ? N2 Eu1 N8 C11 -24.8(3) . . . . ? N7 Eu1 N8 C11 -150.7(3) . . . . ? N8 Eu1 N9 C12 5.6(2) . . . . ? N4 Eu1 N9 C12 143.8(3) . . . . ? N1 Eu1 N9 C12 -153.2(3) . . . . ? N5 Eu1 N9 C12 -97.4(3) . . . . ? N6 Eu1 N9 C12 -73.3(3) . . . . ? N3 Eu1 N9 C12 78.3(3) . . . . ? N2 Eu1 N9 C12 141.3(3) . . . . ? N7 Eu1 N9 C12 10.6(3) . . . . ? Eu1 N1 C1 C2 47.4(5) . . . . ? C3 N2 C2 C1 -146.5(4) . . . . ? Eu1 N2 C2 C1 -3.9(6) . . . . ? N1 C1 C2 N2 -28.6(6) . . . . ? C2 N2 C3 C4 -172.2(4) . . . . ? Eu1 N2 C3 C4 43.8(5) . . . . ? Eu1 N3 C4 C3 44.9(5) . . . . ? N2 C3 C4 N3 -57.6(5) . . . . ? Eu1 N4 C5 C6 -34.7(4) . . . . ? C7 N5 C6 C5 177.2(3) . . . . ? Eu1 N5 C6 C5 -51.4(4) . . . . ? N4 C5 C6 N5 56.9(4) . . . . ? C6 N5 C7 C8 177.8(3) . . . . ? Eu1 N5 C7 C8 47.6(4) . . . . ? Eu1 N6 C8 C7 39.4(4) . . . . ? N5 C7 C8 N6 -56.7(5) . . . . ? Eu1 N7 C9 C10 43.1(4) . . . . ? C11 N8 C10 C9 178.9(3) . . . . ? Eu1 N8 C10 C9 45.0(4) . . . . ? N7 C9 C10 N8 -57.9(4) . . . . ? C10 N8 C11 C12 171.8(4) . . . . ? Eu1 N8 C11 C12 -52.8(4) . . . . ? Eu1 N9 C12 C11 -35.0(4) . . . . ? N8 C11 C12 N9 57.4(5) . . . . ? S1 Ge1 S3 Ge1 -117.29(4) . . . 3_656 ? S2 Ge1 S3 Ge1 114.52(5) . . . 3_656 ? S3 Ge1 S3 Ge1 0.0 3_656 . . 3_656 ? 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 S3 0.90 2.94 3.696(4) 143.2 2_656 N1 H1B Cl1 0.90 2.69 3.422(4) 139.5 2_656 N2 H2C N9 0.91 2.58 3.097(5) 117.1 . N2 H2C S1 0.91 2.66 3.530(4) 159.6 4_666 N3 H3A S2 0.90 2.57 3.472(4) 174.9 3_656 N4 H4A S2 0.90 2.50 3.402(4) 175.1 3_656 N4 H4B Cl1 0.90 2.60 3.398(4) 147.6 4_665 N5 H5C S1 0.91 2.66 3.453(3) 145.7 1_655 N5 H5C N7 0.91 2.70 3.162(5) 112.5 . N6 H6A S2 0.90 2.51 3.358(3) 158.2 2_656 N6 H6B Cl1 0.90 2.54 3.427(3) 170.4 1_655 N7 H7A S2 0.90 2.95 3.783(4) 154.7 3_656 N8 H8C Cl1 0.91 2.42 3.285(3) 160.0 1_655 N8 H8C N6 0.91 2.65 3.124(4) 113.6 . N9 H9A S2 0.90 2.53 3.386(4) 159.8 2_656 N9 H9B S1 0.90 2.61 3.476(3) 162.6 4_666 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.142 _refine_diff_density_min -1.159 _refine_diff_density_rms 0.116 # Attachment 'ce-art-01-2012-025082-File007-v1-0.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 860865' #TrackingRef 'ce-art-01-2012-025082-File007-v1-0.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C8 H24 N5 O S3 Sn Y), (C4 H11.50 N2.50), H2 O' _chemical_formula_sum 'C20 H61.5 N12.5 O3 S6 Sn2 Y2' _chemical_formula_weight 1132.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.638(4) _cell_length_b 14.415(3) _cell_length_c 16.910(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.47(3) _cell_angle_gamma 90.00 _cell_volume 4038.6(19) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 25.10 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 4.420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2814 _exptl_absorpt_correction_T_max 0.4576 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10046 _diffrn_reflns_av_R_equivalents 0.1287 _diffrn_reflns_av_sigmaI/netI 0.2525 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3594 _reflns_number_gt 1444 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0963P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3594 _refine_ls_number_parameters 172 _refine_ls_number_restraints 246 _refine_ls_R_factor_all 0.1715 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1976 _refine_ls_wR_factor_gt 0.1746 _refine_ls_goodness_of_fit_ref 0.853 _refine_ls_restrained_S_all 0.846 _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 Y1 Y 0.20937(6) 0.83048(10) 0.39904(7) 0.0416(4) Uani 1 1 d . . . Ge1 Ge 0.07806(7) 0.96107(11) 0.50917(8) 0.0436(5) Uani 1 1 d . . . S3 S 0.06818(16) 0.8606(3) 0.4061(2) 0.0477(10) Uani 1 1 d . . . S2 S 0.00046(18) 1.0884(3) 0.4369(2) 0.0517(10) Uani 1 1 d . . . S1 S 0.20025(18) 0.9992(3) 0.6186(2) 0.0608(12) Uani 1 1 d . . . O1 O 0.2350(4) 0.6800(6) 0.4419(5) 0.048(2) Uani 1 1 d U . . N1 N 0.0976(6) 0.7412(9) 0.2595(6) 0.066(3) Uani 1 1 d U . . H1A H 0.0812 0.6950 0.2811 0.079 Uiso 1 1 calc R . . H1B H 0.0554 0.7796 0.2261 0.079 Uiso 1 1 calc R . . N2 N 0.2426(7) 0.8022(9) 0.2713(7) 0.076(3) Uani 1 1 d U . . H2C H 0.2408 0.8597 0.2480 0.091 Uiso 1 1 calc R . . N3 N 0.3593(6) 0.8384(9) 0.4595(8) 0.070(3) Uani 1 1 d U . . H3C H 0.3806 0.7873 0.4965 0.084 Uiso 1 1 calc R . . N4 N 0.2648(7) 0.9962(9) 0.4524(9) 0.083(3) Uani 1 1 d U . . H4C H 0.2617 1.0084 0.5031 0.099 Uiso 1 1 calc R . . N5 N 0.1284(7) 0.9533(9) 0.2748(7) 0.070(3) Uani 1 1 d U . . H5A H 0.1445 0.9552 0.2340 0.084 Uiso 1 1 calc R . . H5B H 0.0757 0.9379 0.2427 0.084 Uiso 1 1 calc R . . C1 C 0.1188(10) 0.7026(14) 0.1983(12) 0.104(4) Uani 1 1 d U . . H1C H 0.1393 0.6403 0.2196 0.125 Uiso 1 1 calc R . . H1D H 0.0703 0.6974 0.1362 0.125 Uiso 1 1 calc R . . C2 C 0.1747(10) 0.7513(13) 0.1915(11) 0.099(4) Uani 1 1 d U . . H2A H 0.1451 0.7964 0.1418 0.119 Uiso 1 1 calc R . . H2B H 0.1987 0.7082 0.1692 0.119 Uiso 1 1 calc R . . C3 C 0.3248(9) 0.7727(13) 0.3122(11) 0.088(4) Uani 1 1 d U . . H3A H 0.3298 0.7091 0.3335 0.106 Uiso 1 1 calc R . . H3B H 0.3377 0.7737 0.2644 0.106 Uiso 1 1 calc R . . C4 C 0.3803(8) 0.8272(12) 0.3872(11) 0.085(4) Uani 1 1 d U . . H4A H 0.3828 0.8879 0.3641 0.102 Uiso 1 1 calc R . . H4B H 0.4334 0.7991 0.4160 0.102 Uiso 1 1 calc R . . C5 C 0.3994(9) 0.9152(13) 0.5223(12) 0.096(4) Uani 1 1 d U . . H5C H 0.4523 0.9233 0.5317 0.115 Uiso 1 1 calc R . . H5D H 0.4069 0.9011 0.5825 0.115 Uiso 1 1 calc R . . C6 C 0.3542(9) 1.0011(13) 0.4866(13) 0.109(5) Uani 1 1 d U . . H6A H 0.3586 1.0224 0.4352 0.131 Uiso 1 1 calc R . . H6B H 0.3795 1.0474 0.5358 0.131 Uiso 1 1 calc R . . C7 C 0.2161(10) 1.0699(13) 0.3815(12) 0.111(5) Uani 1 1 d U . . H7A H 0.2152 1.1247 0.4142 0.133 Uiso 1 1 calc R . . H7B H 0.2427 1.0865 0.3491 0.133 Uiso 1 1 calc R . . C8 C 0.1390(10) 1.0449(13) 0.3171(12) 0.099(5) Uani 1 1 d U . . H8A H 0.1159 1.0908 0.2674 0.119 Uiso 1 1 calc R . . H8B H 0.1082 1.0467 0.3468 0.119 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 Y1 0.0361(6) 0.0608(11) 0.0275(6) 0.0022(7) 0.0168(5) 0.0053(6) Ge1 0.0317(7) 0.0686(12) 0.0276(7) -0.0039(7) 0.0140(6) 0.0062(7) S3 0.0313(16) 0.075(3) 0.0310(16) -0.0132(17) 0.0127(14) 0.0075(16) S2 0.0462(19) 0.072(3) 0.0404(19) 0.0074(19) 0.0256(16) 0.0082(18) S1 0.0388(18) 0.085(3) 0.046(2) -0.022(2) 0.0146(16) 0.0030(18) O1 0.043(4) 0.074(6) 0.027(4) 0.000(4) 0.020(3) 0.010(4) N1 0.063(5) 0.106(8) 0.040(5) -0.010(5) 0.034(4) 0.011(5) N2 0.075(5) 0.111(7) 0.055(5) -0.006(5) 0.044(4) -0.002(5) N3 0.058(5) 0.095(7) 0.070(6) 0.003(5) 0.042(4) 0.008(5) N4 0.069(6) 0.080(7) 0.080(6) -0.004(6) 0.028(5) -0.015(6) N5 0.074(6) 0.086(7) 0.052(5) -0.003(5) 0.035(5) -0.002(6) C1 0.085(7) 0.128(9) 0.083(7) -0.032(7) 0.035(6) 0.001(7) C2 0.105(7) 0.122(8) 0.070(6) -0.019(7) 0.048(6) -0.014(7) C3 0.086(6) 0.108(8) 0.081(6) -0.007(6) 0.052(5) 0.013(6) C4 0.065(6) 0.111(8) 0.087(7) 0.006(7) 0.047(6) -0.002(6) C5 0.067(7) 0.102(8) 0.099(7) 0.011(7) 0.031(6) -0.008(7) C6 0.080(7) 0.102(8) 0.103(8) 0.009(7) 0.021(7) -0.017(7) C7 0.092(8) 0.084(9) 0.102(8) 0.008(7) 0.017(7) -0.018(7) C8 0.098(8) 0.100(9) 0.072(8) 0.001(8) 0.027(7) -0.007(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 Y1 O1 2.257(9) . ? Y1 O1 2.302(7) 7_566 ? Y1 N1 2.545(10) . ? Y1 N3 2.548(10) . ? Y1 N5 2.548(11) . ? Y1 N4 2.579(12) . ? Y1 N2 2.602(9) . ? Y1 S3 2.872(3) . ? Y1 Y1 3.707(3) 7_566 ? Ge1 S1 2.172(3) . ? Ge1 S3 2.192(3) . ? Ge1 S2 2.277(4) . ? Ge1 S2 2.287(3) 5_576 ? S2 Ge1 2.287(3) 5_576 ? O1 Y1 2.302(7) 7_566 ? N1 C1 1.420(17) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.438(16) . ? N2 C2 1.484(17) . ? N2 H2C 0.9100 . ? N3 C5 1.440(18) . ? N3 C4 1.495(16) . ? N3 H3C 0.9100 . ? N4 C7 1.499(19) . ? N4 C6 1.526(17) . ? N4 H4C 0.9100 . ? N5 C8 1.463(18) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? C1 C2 1.36(2) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.390(19) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.45(2) . ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.356(19) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y1 O1 71.2(3) . 7_566 ? O1 Y1 N1 75.2(3) . . ? O1 Y1 N1 133.0(3) 7_566 . ? O1 Y1 N3 84.5(3) . . ? O1 Y1 N3 79.2(3) 7_566 . ? N1 Y1 N3 129.0(3) . . ? O1 Y1 N5 150.0(3) . . ? O1 Y1 N5 134.7(3) 7_566 . ? N1 Y1 N5 75.0(4) . . ? N3 Y1 N5 112.0(4) . . ? O1 Y1 N4 143.0(3) . . ? O1 Y1 N4 78.8(4) 7_566 . ? N1 Y1 N4 141.7(4) . . ? N3 Y1 N4 68.8(4) . . ? N5 Y1 N4 66.7(4) . . ? O1 Y1 N2 90.2(3) . . ? O1 Y1 N2 141.9(3) 7_566 . ? N1 Y1 N2 68.1(3) . . ? N3 Y1 N2 65.8(4) . . ? N5 Y1 N2 75.4(4) . . ? N4 Y1 N2 100.9(4) . . ? O1 Y1 S3 100.74(19) . . ? O1 Y1 S3 79.85(18) 7_566 . ? N1 Y1 S3 75.2(2) . . ? N3 Y1 S3 155.5(3) . . ? N5 Y1 S3 74.9(3) . . ? N4 Y1 S3 94.6(3) . . ? N2 Y1 S3 137.4(3) . . ? O1 Y1 Y1 36.01(17) . 7_566 ? O1 Y1 Y1 35.2(2) 7_566 7_566 ? N1 Y1 Y1 105.6(3) . 7_566 ? N3 Y1 Y1 79.9(3) . 7_566 ? N5 Y1 Y1 164.6(2) . 7_566 ? N4 Y1 Y1 111.4(3) . 7_566 ? N2 Y1 Y1 119.4(3) . 7_566 ? S3 Y1 Y1 90.23(8) . 7_566 ? S1 Ge1 S3 115.47(13) . . ? S1 Ge1 S2 111.62(15) . . ? S3 Ge1 S2 110.94(13) . . ? S1 Ge1 S2 114.35(13) . 5_576 ? S3 Ge1 S2 108.69(14) . 5_576 ? S2 Ge1 S2 93.73(13) . 5_576 ? Ge1 S3 Y1 117.24(13) . . ? Ge1 S2 Ge1 86.27(13) . 5_576 ? Y1 O1 Y1 108.8(3) . 7_566 ? C1 N1 Y1 115.5(9) . . ? C1 N1 H1A 108.4 . . ? Y1 N1 H1A 108.4 . . ? C1 N1 H1B 108.4 . . ? Y1 N1 H1B 108.4 . . ? H1A N1 H1B 107.5 . . ? C3 N2 C2 121.3(13) . . ? C3 N2 Y1 111.3(8) . . ? C2 N2 Y1 109.2(8) . . ? C3 N2 H2C 104.5 . . ? C2 N2 H2C 104.5 . . ? Y1 N2 H2C 104.5 . . ? C5 N3 C4 113.8(12) . . ? C5 N3 Y1 112.8(9) . . ? C4 N3 Y1 115.8(8) . . ? C5 N3 H3C 104.3 . . ? C4 N3 H3C 104.3 . . ? Y1 N3 H3C 104.3 . . ? C7 N4 C6 112.4(13) . . ? C7 N4 Y1 114.1(9) . . ? C6 N4 Y1 111.0(10) . . ? C7 N4 H4C 106.2 . . ? C6 N4 H4C 106.2 . . ? Y1 N4 H4C 106.2 . . ? C8 N5 Y1 111.2(9) . . ? C8 N5 H5A 109.4 . . ? Y1 N5 H5A 109.4 . . ? C8 N5 H5B 109.4 . . ? Y1 N5 H5B 109.4 . . ? H5A N5 H5B 108.0 . . ? C2 C1 N1 115.1(16) . . ? C2 C1 H1C 108.5 . . ? N1 C1 H1C 108.5 . . ? C2 C1 H1D 108.5 . . ? N1 C1 H1D 108.5 . . ? H1C C1 H1D 107.5 . . ? C1 C2 N2 123.4(14) . . ? C1 C2 H2A 106.5 . . ? N2 C2 H2A 106.5 . . ? C1 C2 H2B 106.5 . . ? N2 C2 H2B 106.5 . . ? H2A C2 H2B 106.5 . . ? C4 C3 N2 113.6(14) . . ? C4 C3 H3A 108.8 . . ? N2 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? N2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 N3 112.3(12) . . ? C3 C4 H4A 109.1 . . ? N3 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? N3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? N3 C5 C6 112.2(14) . . ? N3 C5 H5C 109.2 . . ? C6 C5 H5C 109.2 . . ? N3 C5 H5D 109.2 . . ? C6 C5 H5D 109.2 . . ? H5C C5 H5D 107.9 . . ? C5 C6 N4 116.1(14) . . ? C5 C6 H6A 108.3 . . ? N4 C6 H6A 108.3 . . ? C5 C6 H6B 108.3 . . ? N4 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C8 C7 N4 114.3(15) . . ? C8 C7 H7A 108.7 . . ? N4 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? N4 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 N5 115.9(16) . . ? C7 C8 H8A 108.3 . . ? N5 C8 H8A 108.3 . . ? C7 C8 H8B 108.3 . . ? N5 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.055 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.180 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.366 -0.250 0.166 419.1 74.2 2 0.392 0.250 0.641 419.1 74.2 _platon_squeeze_details ; ; ########End