# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Pingyun Feng' _publ_contact_author_address ; Department of Chemistry University of California at Riverside Riverside 92521 UNITED STATES OF AMERICA ; _publ_contact_author_email PINGYUN.FENG@UCR.EDU _publ_section_title ; Two dimensional organization of [ZnGe3S9(H2O]4- supertetrahedral clusters templated by a chiral metal complex ; loop_ _publ_author_name 'Pingyun Feng' 'Xianhui Bu' 'Nanfeng Zheng' data_UCR-28 _database_code_depnum_ccdc_archive 'CCDC 262154' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common UCR-28 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H24 Ge3 N4 O3 S9 Zn3' _chemical_formula_weight 902.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' _cell_length_a 9.6014(10) _cell_length_b 9.6014(10) _cell_length_c 8.3735(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 668.51(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Tetrahedron-like _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 430 _exptl_absorpt_coefficient_mu 6.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5005 _exptl_absorpt_correction_T_max 0.6515 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1k' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'Not measured' _diffrn_reflns_number 4163 _diffrn_reflns_av_R_equivalents 0.0755 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1993 _reflns_number_gt 1793 _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^)+(0.0194P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.032(13) _refine_ls_number_reflns 1993 _refine_ls_number_parameters 85 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0575 _refine_ls_wR_factor_gt 0.0560 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.959 _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 Ge1 Ge 0.47982(6) 0.09373(6) 0.06121(5) 0.01683(12) Uani 1 1 d . . . Zn1 Zn 0.6667 0.3333 0.39471(10) 0.0214(2) Uani 1 3 d S . . Zn2 Zn 0.0000 1.0000 0.30359(11) 0.0203(2) Uani 1 3 d S . . Zn3 Zn 0.3333 -0.3333 0.03121(11) 0.0236(3) Uani 1 3 d S . . S1 S 0.46601(14) 0.07685(14) 0.32190(14) 0.0229(3) Uani 1 1 d . . . S2 S 0.29545(15) -0.12241(14) -0.05434(15) 0.0275(3) Uani 1 1 d . . . S3 S 0.72021(13) 0.14372(14) -0.03025(15) 0.0208(3) Uani 1 1 d . . . O1 O 0.3333 -0.3333 0.2802(9) 0.0452(18) Uani 1 3 d S . . O2 O 0.0000 1.0000 0.0533(10) 0.056(2) Uani 1 3 d S . . O3 O 0.6667 0.3333 0.6417(8) 0.070(2) Uani 1 3 d S . . N1 N 0.0000 1.0000 0.5692(7) 0.0162(15) Uani 1 3 d S . . N2 N 0.0422(5) 0.8113(5) 0.3403(5) 0.0272(10) Uani 1 1 d . . . H2A H -0.0451 0.7189 0.3101 0.033 Uiso 1 1 calc R . . H2B H 0.1253 0.8256 0.2789 0.033 Uiso 1 1 calc R . . C1 C -0.0171(6) 0.8447(6) 0.6172(5) 0.0273(11) Uani 1 1 d . . . H1A H -0.1297 0.7622 0.6131 0.033 Uiso 1 1 calc R . . H1B H 0.0197 0.8520 0.7264 0.033 Uiso 1 1 calc R . . C2 C 0.0788(6) 0.7979(6) 0.5090(6) 0.0289(12) Uani 1 1 d . . . H2C H 0.1928 0.8679 0.5286 0.035 Uiso 1 1 calc R . . H2D H 0.0523 0.6883 0.5316 0.035 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 Ge1 0.0143(2) 0.0134(2) 0.0219(3) -0.00021(19) -0.00051(18) 0.00626(19) Zn1 0.0233(3) 0.0233(3) 0.0177(5) 0.000 0.000 0.01164(16) Zn2 0.0207(3) 0.0207(3) 0.0196(5) 0.000 0.000 0.01036(16) Zn3 0.0175(4) 0.0175(4) 0.0359(6) 0.000 0.000 0.00877(18) S1 0.0226(6) 0.0198(6) 0.0227(6) 0.0020(5) 0.0021(5) 0.0079(5) S2 0.0230(6) 0.0163(6) 0.0424(9) -0.0063(5) -0.0138(5) 0.0092(5) S3 0.0166(6) 0.0184(6) 0.0270(6) -0.0032(5) 0.0012(5) 0.0084(5) O1 0.042(3) 0.042(3) 0.052(4) 0.000 0.000 0.0209(13) O2 0.065(4) 0.065(4) 0.037(5) 0.000 0.000 0.0324(18) O3 0.090(4) 0.090(4) 0.030(4) 0.000 0.000 0.045(2) N1 0.018(2) 0.018(2) 0.012(3) 0.000 0.000 0.0091(11) N2 0.031(2) 0.026(2) 0.030(3) -0.0019(19) 0.0013(19) 0.018(2) C1 0.029(3) 0.026(3) 0.025(2) 0.007(2) 0.002(2) 0.013(2) C2 0.033(3) 0.023(3) 0.032(3) 0.003(2) 0.001(2) 0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 S2 2.1686(13) . ? Ge1 S1 2.1880(14) . ? Ge1 S3 2.2442(13) 3_665 ? Ge1 S3 2.2442(12) . ? Zn1 O3 2.068(7) . ? Zn1 S1 2.3245(12) 2_655 ? Zn1 S1 2.3245(12) 3_665 ? Zn1 S1 2.3245(12) . ? Zn2 N2 2.068(4) . ? Zn2 N2 2.068(4) 3_465 ? Zn2 N2 2.068(4) 2_675 ? Zn2 O2 2.096(8) . ? Zn2 N1 2.224(6) . ? Zn3 O1 2.085(7) . ? Zn3 S2 2.3416(13) 2_545 ? Zn3 S2 2.3417(13) . ? Zn3 S2 2.3416(13) 3_655 ? S3 Ge1 2.2442(13) 2_655 ? N1 C1 1.472(5) 3_465 ? N1 C1 1.472(5) . ? N1 C1 1.472(5) 2_675 ? N2 C2 1.476(6) . ? C1 C2 1.512(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ge1 S1 112.58(5) . . ? S2 Ge1 S3 101.72(5) . 3_665 ? S1 Ge1 S3 111.69(5) . 3_665 ? S2 Ge1 S3 108.21(5) . . ? S1 Ge1 S3 111.97(5) . . ? S3 Ge1 S3 110.16(7) 3_665 . ? O3 Zn1 S1 105.21(4) . 2_655 ? O3 Zn1 S1 105.21(4) . 3_665 ? S1 Zn1 S1 113.38(3) 2_655 3_665 ? O3 Zn1 S1 105.21(4) . . ? S1 Zn1 S1 113.38(3) 2_655 . ? S1 Zn1 S1 113.38(3) 3_665 . ? N2 Zn2 N2 117.83(6) . 3_465 ? N2 Zn2 N2 117.83(6) . 2_675 ? N2 Zn2 N2 117.82(6) 3_465 2_675 ? N2 Zn2 O2 98.56(12) . . ? N2 Zn2 O2 98.56(12) 3_465 . ? N2 Zn2 O2 98.56(12) 2_675 . ? N2 Zn2 N1 81.44(12) . . ? N2 Zn2 N1 81.44(12) 3_465 . ? N2 Zn2 N1 81.44(12) 2_675 . ? O2 Zn2 N1 180.000(2) . . ? O1 Zn3 S2 107.81(4) . 2_545 ? O1 Zn3 S2 107.81(4) . . ? S2 Zn3 S2 111.08(3) 2_545 . ? O1 Zn3 S2 107.81(4) . 3_655 ? S2 Zn3 S2 111.08(3) 2_545 3_655 ? S2 Zn3 S2 111.08(3) . 3_655 ? Ge1 S1 Zn1 101.29(5) . . ? Ge1 S2 Zn3 106.60(5) . . ? Ge1 S3 Ge1 107.80(5) 2_655 . ? C1 N1 C1 112.8(2) 3_465 . ? C1 N1 C1 112.8(2) 3_465 2_675 ? C1 N1 C1 112.8(2) . 2_675 ? C1 N1 Zn2 105.8(3) 3_465 . ? C1 N1 Zn2 105.8(3) . . ? C1 N1 Zn2 105.8(3) 2_675 . ? C2 N2 Zn2 112.2(3) . . ? N1 C1 C2 111.2(4) . . ? N2 C2 C1 109.9(4) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.741 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.111