data_global # start Validation Reply Form _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: It is no Acta Cryst. publication. ; # end Validation Reply Form #Added by publCIF (CCDC output) (Di 13. Apr 11:31:01 2010) _audit_update_record ; 2010-04-13 # Formatted by publCIF ; # 1. SUBMISSION DETAILS _publ_contact_author ; Matthias Westerhausen Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 07743 Jena Germany ; _publ_contact_author_phone '03641 948 110' _publ_contact_author_fax '03641 948 102' _publ_contact_author_email m.we@uni-jena.de _publ_requested_journal 'Organometallics' # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Dinuclear Zinc Alkynyls and their Use in the Catalytic Silicon-Carbon Bond Formation ; loop_ _publ_author_name _publ_author_address 'Matthias Westerhausen' ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; 'Marcel Kahnes ' ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena August-Bebel-Str. 2 D-07743 Jena Germany ; 'Helmar G\"orls' ; Institut f\"ur anorganische und analytische Chemie Friedrich-Schiller-Universit\"at Jena Lessing-Str. 8 D-07743 Jena Germany ; # data_FO3951 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H34 N6 Zn2' _chemical_formula_sum 'C40 H34 N6 Zn2' _chemical_formula_weight 729.47 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthrhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.9024(2) _cell_length_b 14.0656(4) _cell_length_c 24.2369(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3375.79(14) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 19563 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.460 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19563 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3865 _reflns_number_gt 2811 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0406P)^2^+0.6522P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3865 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Zn1 Zn -0.02989(2) 0.071047(17) 0.041913(10) 0.01552(9) Uani 1 1 d . . . N1 N -0.15931(17) 0.14682(12) -0.01787(7) 0.0178(4) Uani 1 1 d . . . N2 N 0.08749(18) 0.07009(12) -0.02992(7) 0.0168(4) Uani 1 1 d . . . N3 N 0.17769(18) 0.06165(12) 0.07520(8) 0.0190(4) Uani 1 1 d . . . C1 C -0.2886(2) 0.17176(15) -0.00893(11) 0.0213(5) Uani 1 1 d . . . H1 H -0.315(2) 0.1670(17) 0.0270(10) 0.022(6) Uiso 1 1 d . . . C2 C -0.3725(3) 0.20335(17) -0.05018(11) 0.0282(6) Uani 1 1 d . . . H2 H -0.460(3) 0.222(2) -0.0431(10) 0.031(7) Uiso 1 1 d . . . C3 C -0.3206(3) 0.21036(17) -0.10278(11) 0.0304(6) Uani 1 1 d . . . H3 H -0.375(2) 0.2326(16) -0.1313(10) 0.024(6) Uiso 1 1 d . . . C4 C -0.1881(3) 0.18549(17) -0.11252(11) 0.0264(6) Uani 1 1 d . . . H4 H -0.154(2) 0.1876(16) -0.1460(10) 0.017(6) Uiso 1 1 d . . . C5 C -0.1088(2) 0.15338(15) -0.06881(9) 0.0185(5) Uani 1 1 d . . . C6 C 0.0381(2) 0.12742(18) -0.07599(10) 0.0217(5) Uani 1 1 d . . . H6A H 0.041(2) 0.0950(17) -0.1111(10) 0.020(6) Uiso 1 1 d . . . H6B H 0.090(2) 0.1896(18) -0.0781(10) 0.031(7) Uiso 1 1 d . . . C7 C 0.2325(2) 0.07975(18) -0.02257(9) 0.0194(5) Uani 1 1 d . . . H7B H 0.281(2) 0.0332(18) -0.0426(9) 0.021(6) Uiso 1 1 d . . . H7A H 0.264(2) 0.1456(18) -0.0351(9) 0.018(6) Uiso 1 1 d . . . C8 C 0.2750(2) 0.07041(15) 0.03723(9) 0.0195(5) Uani 1 1 d . . . C9 C 0.4108(2) 0.07442(17) 0.05251(10) 0.0257(6) Uani 1 1 d . . . H9 H 0.475(2) 0.0823(17) 0.0227(11) 0.025(7) Uiso 1 1 d . . . C10 C 0.4452(3) 0.07231(18) 0.10745(12) 0.0307(6) Uani 1 1 d . . . H10 H 0.538(3) 0.0797(18) 0.1173(12) 0.039(8) Uiso 1 1 d . . . C11 C 0.3444(3) 0.06506(17) 0.14661(11) 0.0283(6) Uani 1 1 d . . . H11 H 0.366(2) 0.0658(17) 0.1847(11) 0.032(7) Uiso 1 1 d . . . C12 C 0.2124(2) 0.05943(16) 0.12893(10) 0.0242(5) Uani 1 1 d . . . H12 H 0.142(2) 0.0545(15) 0.1549(10) 0.020(6) Uiso 1 1 d . . . C13 C -0.1187(2) 0.13011(17) 0.10796(9) 0.0215(5) Uani 1 1 d . . . C14 C -0.1803(2) 0.17621(17) 0.14174(9) 0.0217(5) Uani 1 1 d . . . C15 C -0.2541(2) 0.23534(17) 0.18012(9) 0.0218(5) Uani 1 1 d . . . C16 C -0.2343(2) 0.33357(19) 0.18094(10) 0.0275(6) Uani 1 1 d . . . H16 H -0.167(2) 0.3598(17) 0.1554(10) 0.028(7) Uiso 1 1 d . . . C17 C -0.3085(3) 0.3912(2) 0.21638(12) 0.0360(7) Uani 1 1 d . . . H17 H -0.297(3) 0.455(2) 0.2163(11) 0.036(8) Uiso 1 1 d . . . C18 C -0.4031(3) 0.3518(2) 0.25109(12) 0.0422(8) Uani 1 1 d . . . H18 H -0.451(3) 0.391(2) 0.2764(13) 0.052(9) Uiso 1 1 d . . . C19 C -0.4234(3) 0.2547(2) 0.25114(12) 0.0403(7) Uani 1 1 d . . . H19 H -0.485(3) 0.2259(19) 0.2738(12) 0.038(8) Uiso 1 1 d . . . C20 C -0.3489(2) 0.1967(2) 0.21609(10) 0.0307(6) Uani 1 1 d . . . H20 H -0.362(2) 0.1306(19) 0.2162(10) 0.030(7) 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 Zn1 0.01410(15) 0.01624(15) 0.01621(14) -0.00191(11) 0.00333(9) -0.00051(10) N1 0.0175(9) 0.0139(10) 0.0220(10) -0.0019(8) 0.0010(8) -0.0011(8) N2 0.0153(9) 0.0159(10) 0.0192(10) 0.0014(8) 0.0028(7) -0.0014(8) N3 0.0191(10) 0.0157(10) 0.0221(10) -0.0013(8) 0.0027(8) -0.0005(7) C1 0.0203(12) 0.0150(12) 0.0285(14) -0.0003(10) -0.0004(10) -0.0008(10) C2 0.0214(13) 0.0172(13) 0.0459(17) -0.0013(11) -0.0057(11) 0.0018(11) C3 0.0360(15) 0.0189(13) 0.0363(16) 0.0001(11) -0.0153(12) 0.0029(12) C4 0.0391(15) 0.0182(13) 0.0218(14) 0.0012(10) -0.0027(11) 0.0011(11) C5 0.0270(12) 0.0084(11) 0.0203(12) -0.0004(9) -0.0006(9) -0.0016(9) C6 0.0230(12) 0.0212(13) 0.0210(13) 0.0012(10) 0.0030(10) -0.0031(10) C7 0.0149(11) 0.0189(13) 0.0243(12) -0.0048(10) 0.0068(9) -0.0019(10) C8 0.0173(11) 0.0129(11) 0.0284(12) -0.0040(10) 0.0029(9) -0.0016(9) C9 0.0165(12) 0.0248(14) 0.0358(15) -0.0075(11) 0.0015(10) -0.0028(11) C10 0.0199(13) 0.0283(14) 0.0440(16) -0.0069(12) -0.0079(11) -0.0015(11) C11 0.0315(14) 0.0247(14) 0.0288(14) 0.0002(11) -0.0104(11) -0.0003(11) C12 0.0264(13) 0.0215(13) 0.0246(13) 0.0012(10) 0.0008(10) -0.0014(10) C13 0.0165(11) 0.0260(13) 0.0220(12) -0.0018(10) 0.0013(9) -0.0009(10) C14 0.0161(12) 0.0310(14) 0.0179(12) -0.0016(10) -0.0016(9) -0.0010(10) C15 0.0142(11) 0.0365(15) 0.0146(11) -0.0070(10) -0.0045(9) 0.0047(10) C16 0.0226(13) 0.0371(16) 0.0227(13) -0.0051(11) -0.0027(10) 0.0033(11) C17 0.0388(16) 0.0347(17) 0.0345(16) -0.0127(13) -0.0049(12) 0.0076(13) C18 0.0324(16) 0.056(2) 0.0378(17) -0.0250(15) 0.0041(12) 0.0103(15) C19 0.0256(14) 0.063(2) 0.0318(15) -0.0145(14) 0.0094(12) -0.0030(14) C20 0.0244(13) 0.0415(17) 0.0262(14) -0.0108(12) 0.0025(10) -0.0009(13) _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 Zn1 C13 2.007(2) . ? Zn1 N2 2.0858(18) 5 ? Zn1 N2 2.0934(17) . ? Zn1 N1 2.2085(18) . ? Zn1 N3 2.2122(18) . ? Zn1 Zn1 2.9108(5) 5 ? N1 C5 1.335(3) . ? N1 C1 1.345(3) . ? N2 C7 1.453(3) . ? N2 C6 1.462(3) . ? N2 Zn1 2.0858(18) 5 ? N3 C8 1.338(3) . ? N3 C12 1.347(3) . ? C1 C2 1.374(3) . ? C1 H1 0.91(2) . ? C2 C3 1.378(4) . ? C2 H2 0.92(3) . ? C3 C4 1.379(4) . ? C3 H3 0.93(2) . ? C4 C5 1.394(3) . ? C4 H4 0.88(2) . ? C5 C6 1.509(3) . ? C6 H6A 0.97(2) . ? C6 H6B 1.02(2) . ? C7 C8 1.515(3) . ? C7 H7B 0.94(2) . ? C7 H7A 1.02(2) . ? C8 C9 1.396(3) . ? C9 C10 1.375(4) . ? C9 H9 0.97(3) . ? C10 C11 1.381(4) . ? C10 H10 0.96(3) . ? C11 C12 1.378(3) . ? C11 H11 0.95(3) . ? C12 H12 0.94(2) . ? C13 C14 1.210(3) . ? C14 C15 1.446(3) . ? C15 C20 1.392(3) . ? C15 C16 1.396(3) . ? C16 C17 1.391(3) . ? C16 H16 0.98(2) . ? C17 C18 1.376(4) . ? C17 H17 0.90(3) . ? C18 C19 1.380(4) . ? C18 H18 0.95(3) . ? C19 C20 1.389(4) . ? C19 H19 0.91(3) . ? C20 H20 0.94(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Zn1 N2 112.67(8) . 5 ? C13 Zn1 N2 155.44(8) . . ? N2 Zn1 N2 91.71(7) 5 . ? C13 Zn1 N1 93.97(8) . . ? N2 Zn1 N1 102.07(7) 5 . ? N2 Zn1 N1 77.27(7) . . ? C13 Zn1 N3 98.10(8) . . ? N2 Zn1 N3 104.36(7) 5 . ? N2 Zn1 N3 77.70(7) . . ? N1 Zn1 N3 143.83(7) . . ? C13 Zn1 Zn1 158.48(7) . 5 ? N2 Zn1 Zn1 45.96(5) 5 5 ? N2 Zn1 Zn1 45.75(5) . 5 ? N1 Zn1 Zn1 89.51(5) . 5 ? N3 Zn1 Zn1 91.41(5) . 5 ? C5 N1 C1 119.2(2) . . ? C5 N1 Zn1 115.00(14) . . ? C1 N1 Zn1 124.93(16) . . ? C7 N2 C6 111.89(17) . . ? C7 N2 Zn1 112.11(14) . 5 ? C6 N2 Zn1 109.09(14) . 5 ? C7 N2 Zn1 116.50(13) . . ? C6 N2 Zn1 116.47(14) . . ? Zn1 N2 Zn1 88.29(7) 5 . ? C8 N3 C12 118.9(2) . . ? C8 N3 Zn1 114.37(15) . . ? C12 N3 Zn1 126.23(15) . . ? N1 C1 C2 122.9(2) . . ? N1 C1 H1 114.0(15) . . ? C2 C1 H1 123.1(15) . . ? C1 C2 C3 118.1(2) . . ? C1 C2 H2 121.6(16) . . ? C3 C2 H2 120.3(16) . . ? C4 C3 C2 119.7(2) . . ? C4 C3 H3 120.8(14) . . ? C2 C3 H3 119.6(14) . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.9(14) . . ? C5 C4 H4 119.8(14) . . ? N1 C5 C4 120.9(2) . . ? N1 C5 C6 116.78(19) . . ? C4 C5 C6 122.2(2) . . ? N2 C6 C5 111.60(18) . . ? N2 C6 H6A 113.7(14) . . ? C5 C6 H6A 104.1(13) . . ? N2 C6 H6B 110.0(13) . . ? C5 C6 H6B 106.8(13) . . ? H6A C6 H6B 110.3(19) . . ? N2 C7 C8 112.54(18) . . ? N2 C7 H7B 111.9(14) . . ? C8 C7 H7B 106.9(14) . . ? N2 C7 H7A 110.6(12) . . ? C8 C7 H7A 106.1(12) . . ? H7B C7 H7A 108.6(19) . . ? N3 C8 C9 121.0(2) . . ? N3 C8 C7 117.8(2) . . ? C9 C8 C7 121.2(2) . . ? C10 C9 C8 119.7(2) . . ? C10 C9 H9 124.0(15) . . ? C8 C9 H9 116.3(15) . . ? C9 C10 C11 119.2(2) . . ? C9 C10 H10 118.5(17) . . ? C11 C10 H10 122.2(17) . . ? C12 C11 C10 118.4(2) . . ? C12 C11 H11 121.0(15) . . ? C10 C11 H11 120.5(15) . . ? N3 C12 C11 122.8(2) . . ? N3 C12 H12 117.4(14) . . ? C11 C12 H12 119.8(14) . . ? C14 C13 Zn1 169.4(2) . . ? C13 C14 C15 177.1(3) . . ? C20 C15 C16 118.2(2) . . ? C20 C15 C14 121.3(2) . . ? C16 C15 C14 120.5(2) . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H16 122.0(15) . . ? C15 C16 H16 117.3(14) . . ? C18 C17 C16 120.2(3) . . ? C18 C17 H17 119.2(17) . . ? C16 C17 H17 120.6(17) . . ? C17 C18 C19 119.9(3) . . ? C17 C18 H18 119.9(19) . . ? C19 C18 H18 120.2(19) . . ? C18 C19 C20 120.2(3) . . ? C18 C19 H19 122.4(18) . . ? C20 C19 H19 117.3(18) . . ? C19 C20 C15 120.8(3) . . ? C19 C20 H20 120.4(16) . . ? C15 C20 H20 118.8(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.384 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.083 #=== END data_FO3892 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H37 N3 Si2 Zn' _chemical_formula_sum 'C27 H37 N3 Si2 Zn' _chemical_formula_weight 525.15 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' 'Si' 'Si' 0.0817 0.0704 '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' _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 14.9418(4) _cell_length_b 11.6911(3) _cell_length_c 17.1955(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.712(1) _cell_angle_gamma 90.00 _cell_volume 2876.94(13) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 20120 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.956 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20120 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6574 _reflns_number_gt 4908 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0432P)^2^+0.3701P] 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 6574 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 Zn1 Zn 0.554871(14) 0.283844(18) 0.193875(13) 0.02697(8) Uani 1 1 d . . . Si1 Si 0.36607(4) 0.23779(6) 0.24998(4) 0.04039(15) Uani 1 1 d . . . Si2 Si 0.45323(4) 0.04918(5) 0.15869(3) 0.03142(13) Uani 1 1 d . . . N1 N 0.50114(11) 0.44376(14) 0.13740(9) 0.0310(4) Uani 1 1 d . . . N2 N 0.61967(12) 0.40634(14) 0.28795(10) 0.0313(4) Uani 1 1 d . . . N3 N 0.62639(15) 0.26612(17) 0.43457(11) 0.0471(5) Uani 1 1 d . . . C1 C 0.66272(15) 0.26026(17) 0.14916(13) 0.0331(4) Uani 1 1 d . . . C2 C 0.73101(14) 0.24285(17) 0.12581(12) 0.0309(4) Uani 1 1 d . . . C3 C 0.81039(14) 0.21289(16) 0.09849(12) 0.0305(4) Uani 1 1 d . . . C4 C 0.89982(16) 0.2503(2) 0.13946(15) 0.0458(6) Uani 1 1 d . . . H4A H 0.9086 0.3018 0.1837 0.055 Uiso 1 1 calc R . . C5 C 0.97650(17) 0.2127(2) 0.11606(18) 0.0589(7) Uani 1 1 d . . . H5A H 1.0373 0.2384 0.1449 0.071 Uiso 1 1 calc R . . C6 C 0.96552(19) 0.1394(2) 0.05215(19) 0.0623(7) Uani 1 1 d . . . H6A H 1.0182 0.1136 0.0367 0.075 Uiso 1 1 calc R . . C7 C 0.8770(2) 0.1032(2) 0.01046(16) 0.0590(7) Uani 1 1 d . . . H7A H 0.8688 0.0527 -0.0344 0.071 Uiso 1 1 calc R . . C8 C 0.80039(16) 0.1393(2) 0.03293(13) 0.0425(5) Uani 1 1 d . . . H8A H 0.7399 0.1136 0.0033 0.051 Uiso 1 1 calc R . . C9 C 0.42753(15) 0.4634(2) 0.07237(12) 0.0405(5) Uani 1 1 d . . . H9A H 0.3889 0.4008 0.0483 0.049 Uiso 1 1 calc R . . C10 C 0.40592(17) 0.5705(2) 0.03930(14) 0.0491(6) Uani 1 1 d . . . H10A H 0.3537 0.5814 -0.0071 0.059 Uiso 1 1 calc R . . C11 C 0.46113(18) 0.6618(2) 0.07446(15) 0.0511(6) Uani 1 1 d . . . H11A H 0.4479 0.7365 0.0525 0.061 Uiso 1 1 calc R . . C12 C 0.53605(17) 0.64280(19) 0.14212(14) 0.0470(6) Uani 1 1 d . . . H12A H 0.5742 0.7048 0.1681 0.056 Uiso 1 1 calc R . . C13 C 0.55508(15) 0.53265(18) 0.17178(12) 0.0349(5) Uani 1 1 d . . . C14 C 0.63896(15) 0.50444(17) 0.24192(13) 0.0383(5) Uani 1 1 d . . . H14A H 0.6927 0.4865 0.2212 0.046 Uiso 1 1 calc R . . H14B H 0.6558 0.5716 0.2782 0.046 Uiso 1 1 calc R . . C15 C 0.70475(14) 0.36343(19) 0.34851(12) 0.0379(5) Uani 1 1 d . . . H15A H 0.7285 0.4221 0.3910 0.045 Uiso 1 1 calc R . . H15B H 0.7540 0.3480 0.3218 0.045 Uiso 1 1 calc R . . C16 C 0.68248(14) 0.25590(18) 0.38642(12) 0.0355(5) Uani 1 1 d . . . C17 C 0.71533(15) 0.1514(2) 0.36892(14) 0.0442(5) Uani 1 1 d . . . H17A H 0.7547 0.1472 0.3344 0.053 Uiso 1 1 calc R . . C18 C 0.69050(18) 0.0536(2) 0.40190(15) 0.0545(6) Uani 1 1 d . . . H18A H 0.7122 -0.0190 0.3902 0.065 Uiso 1 1 calc R . . C19 C 0.6340(2) 0.0621(2) 0.45180(15) 0.0571(7) Uani 1 1 d . . . H19A H 0.6163 -0.0040 0.4759 0.069 Uiso 1 1 calc R . . C20 C 0.6036(2) 0.1691(2) 0.46608(15) 0.0577(7) Uani 1 1 d . . . H20A H 0.5641 0.1747 0.5004 0.069 Uiso 1 1 calc R . . C21 C 0.46841(13) 0.17447(17) 0.22627(11) 0.0289(4) Uani 1 1 d . . . H21A H 0.5070 0.1442 0.2798 0.035 Uiso 1 1 calc R . . C22 C 0.3286(2) 0.1509(3) 0.32718(18) 0.0682(8) Uani 1 1 d . . . H22A H 0.3798 0.1475 0.3778 0.102 Uiso 1 1 calc R . . H22B H 0.3126 0.0732 0.3063 0.102 Uiso 1 1 calc R . . H22C H 0.2739 0.1866 0.3377 0.102 Uiso 1 1 calc R . . C23 C 0.26207(17) 0.2526(3) 0.15845(18) 0.0655(8) Uani 1 1 d . . . H23A H 0.2427 0.1768 0.1354 0.098 Uiso 1 1 calc R . . H23B H 0.2786 0.3004 0.1178 0.098 Uiso 1 1 calc R . . H23C H 0.2106 0.2882 0.1743 0.098 Uiso 1 1 calc R . . C24 C 0.39085(17) 0.3853(2) 0.29495(16) 0.0520(6) Uani 1 1 d . . . H24A H 0.4439 0.3820 0.3442 0.078 Uiso 1 1 calc R . . H24B H 0.3356 0.4141 0.3086 0.078 Uiso 1 1 calc R . . H24C H 0.4059 0.4366 0.2554 0.078 Uiso 1 1 calc R . . C25 C 0.37560(18) -0.0651(2) 0.18130(16) 0.0539(6) Uani 1 1 d . . . H25A H 0.3989 -0.0872 0.2386 0.081 Uiso 1 1 calc R . . H25B H 0.3757 -0.1319 0.1469 0.081 Uiso 1 1 calc R . . H25C H 0.3118 -0.0356 0.1702 0.081 Uiso 1 1 calc R . . C26 C 0.40398(17) 0.0919(2) 0.04926(13) 0.0482(6) Uani 1 1 d . . . H26A H 0.4426 0.1526 0.0363 0.072 Uiso 1 1 calc R . . H26B H 0.3399 0.1199 0.0400 0.072 Uiso 1 1 calc R . . H26C H 0.4037 0.0255 0.0144 0.072 Uiso 1 1 calc R . . C27 C 0.56916(15) -0.02084(18) 0.16875(13) 0.0386(5) Uani 1 1 d . . . H27A H 0.5962 -0.0468 0.2248 0.058 Uiso 1 1 calc R . . H27B H 0.6114 0.0343 0.1547 0.058 Uiso 1 1 calc R . . H27C H 0.5604 -0.0866 0.1320 0.058 Uiso 1 1 calc R . . H1N2 H 0.5792(16) 0.424(2) 0.3137(13) 0.041(7) 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 Zn1 0.02305(12) 0.02841(13) 0.02936(12) -0.00149(9) 0.00742(9) -0.00168(9) Si1 0.0253(3) 0.0557(4) 0.0434(3) -0.0044(3) 0.0151(3) -0.0009(3) Si2 0.0284(3) 0.0340(3) 0.0313(3) -0.0025(2) 0.0078(2) -0.0076(2) N1 0.0292(8) 0.0335(9) 0.0295(8) -0.0011(7) 0.0072(7) 0.0003(7) N2 0.0269(8) 0.0343(9) 0.0308(8) -0.0034(7) 0.0054(7) 0.0016(7) N3 0.0553(12) 0.0494(12) 0.0371(10) -0.0027(9) 0.0139(9) 0.0045(10) C1 0.0333(11) 0.0289(10) 0.0378(11) -0.0004(9) 0.0114(9) -0.0012(8) C2 0.0328(11) 0.0285(10) 0.0321(10) 0.0037(8) 0.0106(9) -0.0004(8) C3 0.0304(10) 0.0308(10) 0.0331(10) 0.0065(8) 0.0136(8) 0.0032(8) C4 0.0353(12) 0.0549(14) 0.0494(13) -0.0109(11) 0.0156(10) -0.0033(11) C5 0.0309(12) 0.0698(18) 0.0806(19) -0.0080(15) 0.0232(13) -0.0030(12) C6 0.0550(16) 0.0594(17) 0.091(2) -0.0003(15) 0.0495(16) 0.0115(13) C7 0.0730(19) 0.0562(16) 0.0593(15) -0.0130(13) 0.0375(14) 0.0039(14) C8 0.0440(13) 0.0460(13) 0.0406(12) -0.0046(10) 0.0174(10) -0.0026(10) C9 0.0371(12) 0.0443(13) 0.0364(11) 0.0024(10) 0.0047(9) -0.0012(10) C10 0.0469(14) 0.0522(14) 0.0424(12) 0.0119(11) 0.0038(10) 0.0094(12) C11 0.0610(16) 0.0370(13) 0.0538(14) 0.0120(11) 0.0140(12) 0.0100(12) C12 0.0553(14) 0.0292(11) 0.0533(14) -0.0001(10) 0.0104(12) -0.0003(10) C13 0.0358(11) 0.0311(11) 0.0384(10) -0.0020(9) 0.0115(9) 0.0005(9) C14 0.0379(12) 0.0288(11) 0.0426(11) -0.0043(9) 0.0028(9) -0.0042(9) C15 0.0276(10) 0.0425(12) 0.0367(11) -0.0044(10) -0.0017(9) -0.0008(9) C16 0.0270(10) 0.0412(12) 0.0308(10) -0.0032(9) -0.0036(8) 0.0036(9) C17 0.0321(11) 0.0454(13) 0.0508(13) -0.0054(11) 0.0051(10) 0.0075(10) C18 0.0526(15) 0.0429(14) 0.0576(15) -0.0018(12) -0.0010(12) 0.0113(12) C19 0.0703(18) 0.0474(15) 0.0441(13) 0.0126(12) 0.0011(13) -0.0037(13) C20 0.0730(18) 0.0622(17) 0.0409(13) 0.0021(12) 0.0212(13) -0.0029(15) C21 0.0234(9) 0.0353(10) 0.0264(9) 0.0002(8) 0.0049(8) -0.0016(8) C22 0.0646(18) 0.084(2) 0.0743(18) -0.0027(16) 0.0487(16) -0.0110(16) C23 0.0270(12) 0.091(2) 0.0733(19) -0.0099(16) 0.0062(12) 0.0073(13) C24 0.0391(13) 0.0609(16) 0.0634(15) -0.0115(13) 0.0265(12) 0.0099(11) C25 0.0555(15) 0.0495(14) 0.0618(15) -0.0090(12) 0.0250(13) -0.0226(12) C26 0.0471(13) 0.0595(15) 0.0338(11) -0.0050(11) 0.0047(10) -0.0069(12) C27 0.0430(12) 0.0298(11) 0.0443(11) -0.0023(9) 0.0147(10) -0.0007(9) _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 Zn1 C1 1.994(2) . ? Zn1 C21 2.0070(19) . ? Zn1 N1 2.1528(16) . ? Zn1 N2 2.1689(16) . ? Si1 C21 1.8470(19) . ? Si1 C23 1.875(3) . ? Si1 C22 1.880(3) . ? Si1 C24 1.883(3) . ? Si2 C21 1.843(2) . ? Si2 C27 1.878(2) . ? Si2 C25 1.882(2) . ? Si2 C26 1.880(2) . ? N1 C9 1.344(3) . ? N1 C13 1.344(3) . ? N2 C14 1.468(3) . ? N2 C15 1.480(2) . ? N2 H1N2 0.87(2) . ? N3 C16 1.342(3) . ? N3 C20 1.342(3) . ? C1 C2 1.216(3) . ? C2 C3 1.439(3) . ? C3 C4 1.390(3) . ? C3 C8 1.392(3) . ? C4 C5 1.390(3) . ? C4 H4A 0.9500 . ? C5 C6 1.366(4) . ? C5 H5A 0.9500 . ? C6 C7 1.377(4) . ? C6 H6A 0.9500 . ? C7 C8 1.376(3) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 C10 1.375(3) . ? C9 H9A 0.9500 . ? C10 C11 1.377(4) . ? C10 H10A 0.9500 . ? C11 C12 1.381(3) . ? C11 H11A 0.9500 . ? C12 C13 1.384(3) . ? C12 H12A 0.9500 . ? C13 C14 1.505(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.497(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.382(3) . ? C17 C18 1.374(4) . ? C17 H17A 0.9500 . ? C18 C19 1.369(4) . ? C18 H18A 0.9500 . ? C19 C20 1.377(4) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Zn1 C21 132.45(8) . . ? C1 Zn1 N1 100.60(7) . . ? C21 Zn1 N1 119.48(7) . . ? C1 Zn1 N2 98.16(8) . . ? C21 Zn1 N2 113.49(7) . . ? N1 Zn1 N2 77.97(6) . . ? C21 Si1 C23 112.98(11) . . ? C21 Si1 C22 111.88(12) . . ? C23 Si1 C22 107.43(14) . . ? C21 Si1 C24 112.35(10) . . ? C23 Si1 C24 106.14(13) . . ? C22 Si1 C24 105.57(13) . . ? C21 Si2 C27 110.20(9) . . ? C21 Si2 C25 113.92(10) . . ? C27 Si2 C25 106.17(11) . . ? C21 Si2 C26 111.21(10) . . ? C27 Si2 C26 107.04(11) . . ? C25 Si2 C26 107.95(11) . . ? C9 N1 C13 118.54(18) . . ? C9 N1 Zn1 129.33(14) . . ? C13 N1 Zn1 111.99(13) . . ? C14 N2 C15 112.46(16) . . ? C14 N2 Zn1 103.21(12) . . ? C15 N2 Zn1 114.20(13) . . ? C14 N2 H1N2 110.9(15) . . ? C15 N2 H1N2 107.8(15) . . ? Zn1 N2 H1N2 108.2(15) . . ? C16 N3 C20 116.7(2) . . ? C2 C1 Zn1 176.42(18) . . ? C1 C2 C3 175.5(2) . . ? C4 C3 C8 117.95(19) . . ? C4 C3 C2 121.37(19) . . ? C8 C3 C2 120.55(19) . . ? C3 C4 C5 120.4(2) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 120.8(2) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 C7 119.1(2) . . ? C5 C6 H6A 120.4 . . ? C7 C6 H6A 120.4 . . ? C8 C7 C6 120.8(2) . . ? C8 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C7 C8 C3 120.9(2) . . ? C7 C8 H8A 119.6 . . ? C3 C8 H8A 119.6 . . ? N1 C9 C10 122.6(2) . . ? N1 C9 H9A 118.7 . . ? C10 C9 H9A 118.7 . . ? C11 C10 C9 118.9(2) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 118.9(2) . . ? C10 C11 H11A 120.5 . . ? C12 C11 H11A 120.5 . . ? C13 C12 C11 119.4(2) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? N1 C13 C12 121.59(19) . . ? N1 C13 C14 116.05(17) . . ? C12 C13 C14 122.32(19) . . ? N2 C14 C13 110.85(17) . . ? N2 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? N2 C15 C16 109.72(16) . . ? N2 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? N2 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N3 C16 C17 122.5(2) . . ? N3 C16 C15 116.76(19) . . ? C17 C16 C15 120.7(2) . . ? C18 C17 C16 119.4(2) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 119.1(2) . . ? C17 C18 H18A 120.5 . . ? C19 C18 H18A 120.5 . . ? C18 C19 C20 118.2(2) . . ? C18 C19 H19A 120.9 . . ? C20 C19 H19A 120.9 . . ? N3 C20 C19 124.1(3) . . ? N3 C20 H20A 117.9 . . ? C19 C20 H20A 117.9 . . ? Si2 C21 Si1 119.88(10) . . ? Si2 C21 Zn1 107.69(9) . . ? Si1 C21 Zn1 116.47(10) . . ? Si2 C21 H21A 103.5 . . ? Si1 C21 H21A 103.5 . . ? Zn1 C21 H21A 103.5 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.287 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.053 #=== END data_FO3922 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H55 N3 Si4 Zn2' _chemical_formula_sum 'C34 H55 N3 Si4 Zn2' _chemical_formula_weight 748.91 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' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5511(2) _cell_length_b 11.6155(3) _cell_length_c 21.8218(6) _cell_angle_alpha 89.250(2) _cell_angle_beta 89.696(2) _cell_angle_gamma 70.2520(10) _cell_volume 2039.81(9) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 14179 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 27.46 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.318 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14179 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9184 _reflns_number_gt 6431 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0429P)^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 9184 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.005 _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 Zn1 Zn 0.61850(3) 0.61013(2) 0.185990(12) 0.02848(8) Uani 1 1 d . . . Zn2 Zn 0.65484(3) 0.44942(2) 0.293173(12) 0.02789(8) Uani 1 1 d . . . Si1 Si 0.56678(10) 0.88753(6) 0.16859(4) 0.04441(19) Uani 1 1 d . . . Si2 Si 0.40811(9) 0.76052(6) 0.06942(3) 0.03975(18) Uani 1 1 d . . . Si3 Si 0.64624(8) 0.25231(6) 0.39150(3) 0.03561(16) Uani 1 1 d . . . Si4 Si 0.96917(8) 0.20335(6) 0.31005(3) 0.03027(15) Uani 1 1 d . . . N1 N 0.7714(3) 0.46490(18) 0.13250(9) 0.0391(5) Uani 1 1 d . . . N2 N 0.5266(2) 0.47146(16) 0.21332(9) 0.0326(5) Uani 1 1 d . . . N3 N 0.4311(2) 0.58461(17) 0.32104(10) 0.0357(5) Uani 1 1 d . . . C1 C 0.9127(4) 0.4596(3) 0.10421(12) 0.0524(7) Uani 1 1 d . . . H1A H 0.9429 0.5311 0.1024 0.063 Uiso 1 1 calc R . . C2 C 1.0167(4) 0.3537(3) 0.07749(14) 0.0705(10) Uani 1 1 d . . . H2A H 1.1169 0.3520 0.0579 0.085 Uiso 1 1 calc R . . C3 C 0.9710(5) 0.2518(3) 0.08016(15) 0.0750(12) Uani 1 1 d . . . H3A H 1.0389 0.1782 0.0616 0.090 Uiso 1 1 calc R . . C4 C 0.8278(4) 0.2555(3) 0.10942(13) 0.0611(9) Uani 1 1 d . . . H4A H 0.7963 0.1846 0.1117 0.073 Uiso 1 1 calc R . . C5 C 0.7286(3) 0.3638(2) 0.13579(11) 0.0420(7) Uani 1 1 d . . . C6 C 0.5694(3) 0.3749(2) 0.16792(12) 0.0453(7) Uani 1 1 d . . . H6A H 0.4788 0.3925 0.1374 0.054 Uiso 1 1 calc R . . H6B H 0.5799 0.2961 0.1884 0.054 Uiso 1 1 calc R . . C7 C 0.3476(3) 0.5150(2) 0.22777(13) 0.0452(7) Uani 1 1 d . . . H7A H 0.3131 0.4447 0.2399 0.054 Uiso 1 1 calc R . . H7B H 0.2833 0.5541 0.1909 0.054 Uiso 1 1 calc R . . C8 C 0.3115(3) 0.6051(2) 0.27882(12) 0.0401(6) Uani 1 1 d . . . C9 C 0.1652(3) 0.7064(3) 0.28314(15) 0.0555(8) Uani 1 1 d . . . H9A H 0.0806 0.7212 0.2531 0.067 Uiso 1 1 calc R . . C10 C 0.1467(4) 0.7841(3) 0.33199(16) 0.0617(9) Uani 1 1 d . . . H10A H 0.0484 0.8532 0.3356 0.074 Uiso 1 1 calc R . . C11 C 0.2682(4) 0.7624(2) 0.37504(15) 0.0552(8) Uani 1 1 d . . . H11A H 0.2558 0.8150 0.4090 0.066 Uiso 1 1 calc R . . C12 C 0.4092(3) 0.6622(2) 0.36790(12) 0.0425(6) Uani 1 1 d . . . H12A H 0.4952 0.6471 0.3975 0.051 Uiso 1 1 calc R . . C13 C 0.7623(3) 0.5990(2) 0.26219(11) 0.0330(5) Uani 1 1 d . . . C14 C 0.8182(3) 0.6112(2) 0.31219(11) 0.0319(5) Uani 1 1 d . . . C15 C 0.8782(3) 0.6327(2) 0.37134(11) 0.0329(5) Uani 1 1 d . . . C16 C 1.0218(3) 0.5506(2) 0.39708(12) 0.0371(6) Uani 1 1 d . . . H16A H 1.0810 0.4773 0.3763 0.045 Uiso 1 1 calc R . . C17 C 1.0790(3) 0.5756(2) 0.45313(12) 0.0436(6) Uani 1 1 d . . . H17A H 1.1772 0.5194 0.4705 0.052 Uiso 1 1 calc R . . C18 C 0.9939(3) 0.6818(2) 0.48365(12) 0.0460(7) Uani 1 1 d . . . H18A H 1.0339 0.6985 0.5219 0.055 Uiso 1 1 calc R . . C19 C 0.8514(4) 0.7632(2) 0.45880(12) 0.0460(7) Uani 1 1 d . . . H19A H 0.7926 0.8360 0.4800 0.055 Uiso 1 1 calc R . . C20 C 0.7930(3) 0.7396(2) 0.40296(12) 0.0409(6) Uani 1 1 d . . . H20A H 0.6946 0.7965 0.3860 0.049 Uiso 1 1 calc R . . C21 C 0.4736(3) 0.77064(19) 0.14855(10) 0.0312(5) Uani 1 1 d . . . H21A H 0.3684 0.7932 0.1729 0.037 Uiso 1 1 calc R . . C22 C 0.7939(4) 0.8356(3) 0.14973(16) 0.0701(9) Uani 1 1 d . . . H22A H 0.8519 0.7608 0.1731 0.105 Uiso 1 1 calc R . . H22B H 0.8392 0.8997 0.1604 0.105 Uiso 1 1 calc R . . H22C H 0.8093 0.8190 0.1058 0.105 Uiso 1 1 calc R . . C23 C 0.4733(5) 1.0408(3) 0.12838(18) 0.0843(12) Uani 1 1 d . . . H23A H 0.3526 1.0707 0.1344 0.126 Uiso 1 1 calc R . . H23B H 0.4982 1.0315 0.0845 0.126 Uiso 1 1 calc R . . H23C H 0.5206 1.0994 0.1454 0.126 Uiso 1 1 calc R . . C24 C 0.5377(4) 0.9200(3) 0.25230(14) 0.0662(9) Uani 1 1 d . . . H24A H 0.5776 0.8430 0.2756 0.099 Uiso 1 1 calc R . . H24B H 0.4195 0.9615 0.2609 0.099 Uiso 1 1 calc R . . H24C H 0.6007 0.9727 0.2642 0.099 Uiso 1 1 calc R . . C25 C 0.5840(4) 0.7357(3) 0.01425(13) 0.0665(9) Uani 1 1 d . . . H25A H 0.6709 0.6575 0.0236 0.100 Uiso 1 1 calc R . . H25B H 0.6295 0.8023 0.0178 0.100 Uiso 1 1 calc R . . H25C H 0.5437 0.7344 -0.0276 0.100 Uiso 1 1 calc R . . C26 C 0.3277(4) 0.6307(3) 0.05879(15) 0.0680(10) Uani 1 1 d . . . H26A H 0.4156 0.5533 0.0687 0.102 Uiso 1 1 calc R . . H26B H 0.2930 0.6298 0.0161 0.102 Uiso 1 1 calc R . . H26C H 0.2325 0.6412 0.0860 0.102 Uiso 1 1 calc R . . C27 C 0.2344(4) 0.9021(2) 0.04380(14) 0.0623(9) Uani 1 1 d . . . H27A H 0.1378 0.9145 0.0706 0.093 Uiso 1 1 calc R . . H27B H 0.2039 0.8921 0.0015 0.093 Uiso 1 1 calc R . . H27C H 0.2713 0.9731 0.0461 0.093 Uiso 1 1 calc R . . C28 C 0.7880(3) 0.31399(18) 0.34865(10) 0.0273(5) Uani 1 1 d . . . H28A H 0.8362 0.3542 0.3801 0.033 Uiso 1 1 calc R . . C29 C 0.4822(4) 0.2368(3) 0.33850(15) 0.0640(9) Uani 1 1 d . . . H29A H 0.4001 0.3178 0.3302 0.096 Uiso 1 1 calc R . . H29B H 0.4270 0.1841 0.3577 0.096 Uiso 1 1 calc R . . H29C H 0.5338 0.2006 0.2999 0.096 Uiso 1 1 calc R . . C30 C 0.7434(4) 0.0998(2) 0.43047(15) 0.0601(8) Uani 1 1 d . . . H30A H 0.8305 0.1040 0.4585 0.090 Uiso 1 1 calc R . . H30B H 0.7920 0.0373 0.3996 0.090 Uiso 1 1 calc R . . H30C H 0.6583 0.0787 0.4537 0.090 Uiso 1 1 calc R . . C31 C 0.5396(4) 0.3576(2) 0.45429(13) 0.0533(7) Uani 1 1 d . . . H31A H 0.6223 0.3641 0.4837 0.080 Uiso 1 1 calc R . . H31B H 0.4611 0.3254 0.4752 0.080 Uiso 1 1 calc R . . H31C H 0.4793 0.4387 0.4370 0.080 Uiso 1 1 calc R . . C32 C 0.9053(3) 0.0936(2) 0.26194(12) 0.0442(7) Uani 1 1 d . . . H32A H 0.8258 0.1393 0.2307 0.066 Uiso 1 1 calc R . . H32B H 0.8533 0.0475 0.2881 0.066 Uiso 1 1 calc R . . H32C H 1.0035 0.0367 0.2420 0.066 Uiso 1 1 calc R . . C33 C 1.0793(3) 0.2810(2) 0.25788(12) 0.0399(6) Uani 1 1 d . . . H33A H 1.1094 0.3423 0.2809 0.060 Uiso 1 1 calc R . . H33B H 1.0058 0.3211 0.2239 0.060 Uiso 1 1 calc R . . H33C H 1.1801 0.2201 0.2416 0.060 Uiso 1 1 calc R . . C34 C 1.1263(3) 0.1114(2) 0.36734(12) 0.0401(6) Uani 1 1 d . . . H34A H 1.1629 0.1667 0.3926 0.060 Uiso 1 1 calc R . . H34B H 1.2221 0.0554 0.3457 0.060 Uiso 1 1 calc R . . H34C H 1.0760 0.0643 0.3936 0.060 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 Zn1 0.03204(16) 0.02663(14) 0.02639(15) 0.00072(11) -0.00255(11) -0.00942(12) Zn2 0.02805(15) 0.02507(14) 0.02961(15) 0.00318(11) -0.00442(11) -0.00782(11) Si1 0.0605(5) 0.0330(4) 0.0444(4) 0.0062(3) -0.0082(4) -0.0221(4) Si2 0.0501(4) 0.0314(4) 0.0305(4) 0.0024(3) -0.0075(3) -0.0042(3) Si3 0.0337(4) 0.0294(3) 0.0438(4) 0.0065(3) 0.0021(3) -0.0110(3) Si4 0.0290(3) 0.0269(3) 0.0332(4) 0.0007(3) -0.0042(3) -0.0072(3) N1 0.0419(12) 0.0367(11) 0.0302(11) -0.0015(10) -0.0034(10) -0.0021(10) N2 0.0351(11) 0.0308(10) 0.0348(11) 0.0027(9) -0.0090(9) -0.0149(9) N3 0.0301(11) 0.0318(10) 0.0422(12) 0.0089(10) -0.0002(10) -0.0068(9) C1 0.0499(17) 0.0597(18) 0.0348(15) 0.0014(14) 0.0032(13) -0.0017(14) C2 0.0526(19) 0.092(3) 0.0409(18) -0.0069(19) 0.0037(15) 0.0099(19) C3 0.087(3) 0.057(2) 0.0439(19) -0.0124(17) -0.0135(19) 0.024(2) C4 0.085(2) 0.0410(16) 0.0402(17) -0.0117(14) -0.0177(17) 0.0013(16) C5 0.0578(17) 0.0300(13) 0.0284(13) -0.0050(11) -0.0172(12) -0.0015(12) C6 0.0620(18) 0.0361(14) 0.0426(16) 0.0033(13) -0.0206(14) -0.0226(13) C7 0.0341(14) 0.0556(16) 0.0513(17) 0.0195(14) -0.0151(12) -0.0226(13) C8 0.0309(14) 0.0420(14) 0.0467(16) 0.0180(13) 0.0024(12) -0.0122(12) C9 0.0317(15) 0.0598(18) 0.068(2) 0.0335(17) -0.0009(14) -0.0081(14) C10 0.0520(19) 0.0407(16) 0.078(2) 0.0165(17) 0.0237(18) 0.0024(14) C11 0.060(2) 0.0347(15) 0.062(2) 0.0060(15) 0.0198(17) -0.0045(14) C12 0.0470(16) 0.0330(13) 0.0442(16) 0.0044(13) 0.0109(13) -0.0095(12) C13 0.0326(13) 0.0293(12) 0.0379(14) 0.0019(11) -0.0014(11) -0.0114(10) C14 0.0320(13) 0.0278(12) 0.0387(14) 0.0036(11) -0.0041(11) -0.0137(10) C15 0.0374(14) 0.0322(12) 0.0336(13) 0.0017(11) -0.0035(11) -0.0177(11) C16 0.0384(14) 0.0358(13) 0.0384(15) 0.0018(12) -0.0035(11) -0.0143(12) C17 0.0427(15) 0.0461(15) 0.0412(15) 0.0110(13) -0.0137(12) -0.0144(13) C18 0.0618(18) 0.0496(16) 0.0320(14) 0.0047(13) -0.0141(13) -0.0260(15) C19 0.0637(19) 0.0396(14) 0.0347(15) -0.0017(12) -0.0058(13) -0.0172(14) C20 0.0475(16) 0.0357(14) 0.0372(15) 0.0038(12) -0.0079(12) -0.0111(12) C21 0.0339(13) 0.0278(11) 0.0292(13) 0.0002(10) -0.0006(10) -0.0069(10) C22 0.068(2) 0.083(2) 0.078(2) 0.0095(19) -0.0075(18) -0.0493(19) C23 0.128(3) 0.0418(17) 0.091(3) 0.0167(18) -0.034(2) -0.040(2) C24 0.101(3) 0.0407(16) 0.055(2) -0.0111(15) -0.0147(18) -0.0217(17) C25 0.077(2) 0.071(2) 0.0334(16) 0.0090(15) 0.0058(15) -0.0017(18) C26 0.098(3) 0.0561(18) 0.054(2) 0.0073(16) -0.0404(18) -0.0312(19) C27 0.067(2) 0.0470(16) 0.057(2) 0.0017(15) -0.0263(16) 0.0016(15) C28 0.0292(12) 0.0232(11) 0.0296(12) 0.0030(10) -0.0062(10) -0.0090(9) C29 0.0550(19) 0.072(2) 0.080(2) 0.0082(18) -0.0077(17) -0.0412(17) C30 0.0573(19) 0.0391(15) 0.079(2) 0.0229(15) 0.0141(17) -0.0112(14) C31 0.0527(17) 0.0490(16) 0.0540(18) 0.0079(14) 0.0159(14) -0.0123(14) C32 0.0500(16) 0.0325(13) 0.0474(16) -0.0040(12) -0.0082(13) -0.0102(12) C33 0.0356(14) 0.0435(14) 0.0372(14) 0.0056(12) -0.0007(11) -0.0090(12) C34 0.0291(13) 0.0405(14) 0.0454(15) 0.0037(12) -0.0028(11) -0.0048(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C21 2.022(2) . ? Zn1 C13 2.050(2) . ? Zn1 N2 2.0957(18) . ? Zn1 N1 2.1124(19) . ? Zn1 Zn2 2.9246(4) . ? Zn2 C28 1.998(2) . ? Zn2 N2 2.0305(19) . ? Zn2 N3 2.1163(19) . ? Zn2 C13 2.316(2) . ? Si1 C21 1.849(2) . ? Si1 C24 1.868(3) . ? Si1 C22 1.874(3) . ? Si1 C23 1.893(3) . ? Si2 C21 1.836(2) . ? Si2 C25 1.869(3) . ? Si2 C26 1.874(3) . ? Si2 C27 1.886(3) . ? Si3 C28 1.848(2) . ? Si3 C31 1.866(3) . ? Si3 C30 1.877(3) . ? Si3 C29 1.879(3) . ? Si4 C28 1.852(2) . ? Si4 C34 1.877(3) . ? Si4 C33 1.879(3) . ? Si4 C32 1.881(2) . ? N1 C1 1.337(3) . ? N1 C5 1.343(3) . ? N2 C6 1.456(3) . ? N2 C7 1.475(3) . ? N3 C8 1.338(3) . ? N3 C12 1.342(3) . ? C1 C2 1.385(4) . ? C1 H1A 0.9500 . ? C2 C3 1.368(5) . ? C2 H2A 0.9500 . ? C3 C4 1.366(5) . ? C3 H3A 0.9500 . ? C4 C5 1.388(4) . ? C4 H4A 0.9500 . ? C5 C6 1.495(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.497(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.401(3) . ? C9 C10 1.379(4) . ? C9 H9A 0.9500 . ? C10 C11 1.361(4) . ? C10 H10A 0.9500 . ? C11 C12 1.374(4) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.222(3) . ? C14 C15 1.447(3) . ? C15 C16 1.391(3) . ? C15 C20 1.398(3) . ? C16 C17 1.390(3) . ? C16 H16A 0.9500 . ? C17 C18 1.379(3) . ? C17 H17A 0.9500 . ? C18 C19 1.375(4) . ? C18 H18A 0.9500 . ? C19 C20 1.384(3) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Zn1 C13 123.16(9) . . ? C21 Zn1 N2 122.98(8) . . ? C13 Zn1 N2 95.90(8) . . ? C21 Zn1 N1 122.42(9) . . ? C13 Zn1 N1 102.06(8) . . ? N2 Zn1 N1 80.24(8) . . ? C21 Zn1 Zn2 143.26(7) . . ? C13 Zn1 Zn2 51.95(6) . . ? N2 Zn1 Zn2 43.97(5) . . ? N1 Zn1 Zn2 91.72(6) . . ? C28 Zn2 N2 138.91(8) . . ? C28 Zn2 N3 122.76(9) . . ? N2 Zn2 N3 80.99(8) . . ? C28 Zn2 C13 119.55(9) . . ? N2 Zn2 C13 89.94(8) . . ? N3 Zn2 C13 90.78(8) . . ? C28 Zn2 Zn1 152.38(6) . . ? N2 Zn2 Zn1 45.77(5) . . ? N3 Zn2 Zn1 83.30(6) . . ? C13 Zn2 Zn1 44.19(6) . . ? C21 Si1 C24 109.32(13) . . ? C21 Si1 C22 111.46(12) . . ? C24 Si1 C22 109.37(16) . . ? C21 Si1 C23 115.33(13) . . ? C24 Si1 C23 105.62(15) . . ? C22 Si1 C23 105.45(17) . . ? C21 Si2 C25 111.61(13) . . ? C21 Si2 C26 112.52(13) . . ? C25 Si2 C26 106.46(16) . . ? C21 Si2 C27 112.61(12) . . ? C25 Si2 C27 107.73(15) . . ? C26 Si2 C27 105.49(14) . . ? C28 Si3 C31 110.70(11) . . ? C28 Si3 C30 116.55(12) . . ? C31 Si3 C30 104.65(14) . . ? C28 Si3 C29 109.71(12) . . ? C31 Si3 C29 107.86(14) . . ? C30 Si3 C29 106.95(14) . . ? C28 Si4 C34 111.13(11) . . ? C28 Si4 C33 112.23(11) . . ? C34 Si4 C33 106.85(12) . . ? C28 Si4 C32 111.42(11) . . ? C34 Si4 C32 107.90(11) . . ? C33 Si4 C32 107.06(12) . . ? C1 N1 C5 119.1(2) . . ? C1 N1 Zn1 126.79(19) . . ? C5 N1 Zn1 113.40(17) . . ? C6 N2 C7 111.83(19) . . ? C6 N2 Zn2 120.71(15) . . ? C7 N2 Zn2 108.31(15) . . ? C6 N2 Zn1 110.02(15) . . ? C7 N2 Zn1 114.20(15) . . ? Zn2 N2 Zn1 90.26(7) . . ? C8 N3 C12 119.2(2) . . ? C8 N3 Zn2 112.05(16) . . ? C12 N3 Zn2 127.52(17) . . ? N1 C1 C2 122.5(3) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C3 C2 C1 118.1(3) . . ? C3 C2 H2A 121.0 . . ? C1 C2 H2A 121.0 . . ? C2 C3 C4 120.1(3) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? N1 C5 C4 120.8(3) . . ? N1 C5 C6 116.9(2) . . ? C4 C5 C6 122.3(3) . . ? N2 C6 C5 111.77(19) . . ? N2 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 110.15(19) . . ? N2 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N3 C8 C9 120.7(3) . . ? N3 C8 C7 115.5(2) . . ? C9 C8 C7 123.9(3) . . ? C10 C9 C8 118.6(3) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C12 118.1(3) . . ? C10 C11 H11A 121.0 . . ? C12 C11 H11A 121.0 . . ? N3 C12 C11 123.0(3) . . ? N3 C12 H12A 118.5 . . ? C11 C12 H12A 118.5 . . ? C14 C13 Zn1 166.3(2) . . ? C14 C13 Zn2 96.04(17) . . ? Zn1 C13 Zn2 83.86(8) . . ? C13 C14 C15 176.7(2) . . ? C16 C15 C20 118.9(2) . . ? C16 C15 C14 121.5(2) . . ? C20 C15 C14 119.7(2) . . ? C17 C16 C15 120.1(2) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C18 C17 C16 120.4(2) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C19 C18 C17 120.0(2) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C20 120.3(2) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C15 120.4(2) . . ? C19 C20 H20A 119.8 . . ? C15 C20 H20A 119.8 . . ? Si2 C21 Si1 119.85(13) . . ? Si2 C21 Zn1 114.76(10) . . ? Si1 C21 Zn1 107.29(11) . . ? Si2 C21 H21A 104.4 . . ? Si1 C21 H21A 104.4 . . ? Zn1 C21 H21A 104.4 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si3 C28 Si4 117.65(11) . . ? Si3 C28 Zn2 109.20(11) . . ? Si4 C28 Zn2 113.07(12) . . ? Si3 C28 H28A 105.3 . . ? Si4 C28 H28A 105.3 . . ? Zn2 C28 H28A 105.3 . . ? Si3 C29 H29A 109.5 . . ? Si3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si3 C30 H30A 109.5 . . ? Si3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si4 C32 H32A 109.5 . . ? Si4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si4 C33 H33A 109.5 . . ? Si4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si4 C34 H34A 109.5 . . ? Si4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.321 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.065 #=== END data_FO3978 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H61 N3 O Si4 Zn2' _chemical_formula_sum 'C41 H61 N3 O Si4 Zn2' _chemical_formula_weight 855.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9012(4) _cell_length_b 21.4948(6) _cell_length_c 18.1196(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.497(2) _cell_angle_gamma 90.00 _cell_volume 4635.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 32342 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.53 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32342 _diffrn_reflns_av_R_equivalents 0.1093 _diffrn_reflns_av_sigmaI/netI 0.1252 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.53 _reflns_number_total 10621 _reflns_number_gt 6024 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] 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 10621 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1228 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.0870 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _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 Zn1 Zn 0.86456(3) 0.299008(16) 0.65583(2) 0.02147(11) Uani 1 1 d . . . Zn2 Zn 0.71966(3) 0.187152(15) 0.64557(2) 0.02078(11) Uani 1 1 d . . . Si1 Si 0.76328(8) 0.43598(4) 0.67469(6) 0.0295(2) Uani 1 1 d . . . Si2 Si 1.01981(9) 0.40893(4) 0.71025(7) 0.0414(3) Uani 1 1 d . . . Si3 Si 0.76807(9) 0.06954(4) 0.54433(6) 0.0333(3) Uani 1 1 d . . . Si4 Si 0.59704(8) 0.05803(4) 0.67877(6) 0.0321(3) Uani 1 1 d . . . O1 O 0.78041(17) 0.25173(9) 0.57627(13) 0.0226(5) Uani 1 1 d . . . N1 N 1.0038(2) 0.23257(12) 0.66150(16) 0.0237(6) Uani 1 1 d . . . N2 N 0.8008(2) 0.23584(11) 0.72973(15) 0.0214(6) Uani 1 1 d . . . N3 N 0.5813(2) 0.23921(11) 0.68551(16) 0.0225(6) Uani 1 1 d . . . C1 C 1.0931(3) 0.22475(15) 0.6171(2) 0.0285(8) Uani 1 1 d . . . H1A H 1.1018 0.2522 0.5765 0.034 Uiso 1 1 calc R . . C2 C 1.1720(3) 0.17899(16) 0.6278(2) 0.0340(9) Uani 1 1 d . . . H2A H 1.2334 0.1746 0.5951 0.041 Uiso 1 1 calc R . . C3 C 1.1600(3) 0.13948(16) 0.6872(2) 0.0364(10) Uani 1 1 d . . . H3A H 1.2136 0.1076 0.6964 0.044 Uiso 1 1 calc R . . C4 C 1.0693(3) 0.14687(15) 0.7331(2) 0.0303(9) Uani 1 1 d . . . H4A H 1.0599 0.1201 0.7743 0.036 Uiso 1 1 calc R . . C5 C 0.9917(3) 0.19363(13) 0.71871(19) 0.0227(8) Uani 1 1 d . . . C6 C 0.8925(3) 0.20331(14) 0.7677(2) 0.0257(8) Uani 1 1 d . . . H6A H 0.8652 0.1624 0.7852 0.031 Uiso 1 1 calc R . . H6B H 0.9161 0.2278 0.8115 0.031 Uiso 1 1 calc R . . C7 C 0.7174(3) 0.25265(15) 0.78455(19) 0.0251(8) Uani 1 1 d . . . H7A H 0.7440 0.2895 0.8124 0.030 Uiso 1 1 calc R . . H7B H 0.7089 0.2179 0.8200 0.030 Uiso 1 1 calc R . . C8 C 0.6047(3) 0.26694(14) 0.7499(2) 0.0241(8) Uani 1 1 d . . . C9 C 0.5251(3) 0.30410(14) 0.7846(2) 0.0291(8) Uani 1 1 d . . . H9A H 0.5427 0.3236 0.8303 0.035 Uiso 1 1 calc R . . C10 C 0.4210(3) 0.31246(15) 0.7524(2) 0.0320(9) Uani 1 1 d . . . H10A H 0.3654 0.3369 0.7760 0.038 Uiso 1 1 calc R . . C11 C 0.3987(3) 0.28465(15) 0.6851(2) 0.0320(9) Uani 1 1 d . . . H11A H 0.3281 0.2903 0.6613 0.038 Uiso 1 1 calc R . . C12 C 0.4805(3) 0.24859(14) 0.6531(2) 0.0272(8) Uani 1 1 d . . . H12A H 0.4653 0.2297 0.6067 0.033 Uiso 1 1 calc R . . C13 C 0.8919(3) 0.39121(13) 0.6554(2) 0.0253(8) Uani 1 1 d . . . H13A H 0.9116 0.4016 0.6033 0.030 Uiso 1 1 calc R . . C14 C 0.7365(4) 0.43940(18) 0.7764(2) 0.0508(11) Uani 1 1 d . . . H14A H 0.7989 0.4609 0.8012 0.076 Uiso 1 1 calc R . . H14B H 0.7302 0.3970 0.7960 0.076 Uiso 1 1 calc R . . H14C H 0.6664 0.4620 0.7853 0.076 Uiso 1 1 calc R . . C15 C 0.6336(3) 0.40408(16) 0.6294(2) 0.0364(9) Uani 1 1 d . . . H15A H 0.6312 0.3589 0.6361 0.055 Uiso 1 1 calc R . . H15B H 0.6345 0.4138 0.5766 0.055 Uiso 1 1 calc R . . H15C H 0.5671 0.4229 0.6518 0.055 Uiso 1 1 calc R . . C16 C 0.7735(3) 0.51847(15) 0.6411(2) 0.0399(10) Uani 1 1 d . . . H16A H 0.8378 0.5389 0.6649 0.060 Uiso 1 1 calc R . . H16B H 0.7044 0.5409 0.6533 0.060 Uiso 1 1 calc R . . H16C H 0.7835 0.5186 0.5875 0.060 Uiso 1 1 calc R . . C17 C 1.0369(3) 0.49110(16) 0.7438(2) 0.0456(11) Uani 1 1 d . . . H17A H 0.9742 0.5018 0.7762 0.068 Uiso 1 1 calc R . . H17B H 1.0375 0.5195 0.7015 0.068 Uiso 1 1 calc R . . H17C H 1.1078 0.4949 0.7713 0.068 Uiso 1 1 calc R . . C18 C 1.0280(5) 0.36036(19) 0.7959(3) 0.089(2) Uani 1 1 d . . . H18A H 0.9577 0.3641 0.8232 0.133 Uiso 1 1 calc R . . H18B H 1.0907 0.3748 0.8269 0.133 Uiso 1 1 calc R . . H18C H 1.0401 0.3167 0.7823 0.133 Uiso 1 1 calc R . . C19 C 1.1474(3) 0.39346(19) 0.6521(3) 0.0723(17) Uani 1 1 d . . . H19A H 1.1435 0.4189 0.6073 0.108 Uiso 1 1 calc R . . H19B H 1.1495 0.3493 0.6386 0.108 Uiso 1 1 calc R . . H19C H 1.2154 0.4041 0.6803 0.108 Uiso 1 1 calc R . . C20 C 0.7219(3) 0.09416(14) 0.6362(2) 0.0239(8) Uani 1 1 d . . . H20A H 0.7852 0.0812 0.6694 0.029 Uiso 1 1 calc R . . C21 C 0.6643(4) 0.09282(18) 0.4714(2) 0.0500(11) Uani 1 1 d . . . H21A H 0.5984 0.0656 0.4738 0.075 Uiso 1 1 calc R . . H21B H 0.6990 0.0891 0.4227 0.075 Uiso 1 1 calc R . . H21C H 0.6411 0.1360 0.4795 0.075 Uiso 1 1 calc R . . C22 C 0.9084(3) 0.10525(19) 0.5243(3) 0.0516(12) Uani 1 1 d . . . H22A H 0.9042 0.1504 0.5314 0.077 Uiso 1 1 calc R . . H22B H 0.9291 0.0963 0.4732 0.077 Uiso 1 1 calc R . . H22C H 0.9652 0.0878 0.5578 0.077 Uiso 1 1 calc R . . C23 C 0.7892(4) -0.01693(17) 0.5335(3) 0.0538(12) Uani 1 1 d . . . H23A H 0.7162 -0.0380 0.5356 0.081 Uiso 1 1 calc R . . H23B H 0.8377 -0.0323 0.5735 0.081 Uiso 1 1 calc R . . H23C H 0.8245 -0.0254 0.4859 0.081 Uiso 1 1 calc R . . C24 C 0.4650(3) 0.07422(17) 0.6255(3) 0.0529(13) Uani 1 1 d . . . H24A H 0.4531 0.1193 0.6225 0.079 Uiso 1 1 calc R . . H24B H 0.4012 0.0549 0.6505 0.079 Uiso 1 1 calc R . . H24C H 0.4714 0.0570 0.5757 0.079 Uiso 1 1 calc R . . C25 C 0.5764(4) 0.0875(2) 0.7746(3) 0.0635(14) Uani 1 1 d . . . H25A H 0.5609 0.1322 0.7731 0.095 Uiso 1 1 calc R . . H25B H 0.6446 0.0799 0.8040 0.095 Uiso 1 1 calc R . . H25C H 0.5129 0.0658 0.7971 0.095 Uiso 1 1 calc R . . C26 C 0.6077(3) -0.02911(16) 0.6873(3) 0.0517(12) Uani 1 1 d . . . H26A H 0.5999 -0.0481 0.6383 0.078 Uiso 1 1 calc R . . H26B H 0.5478 -0.0444 0.7193 0.078 Uiso 1 1 calc R . . H26C H 0.6809 -0.0402 0.7086 0.078 Uiso 1 1 calc R . . C27 C 0.7631(3) 0.26142(15) 0.5000(2) 0.0283(8) Uani 1 1 d . . . H27A H 0.7974 0.2255 0.4733 0.034 Uiso 1 1 calc R . . C28 C 0.6416(3) 0.26245(15) 0.4813(2) 0.0293(8) Uani 1 1 d . . . C29 C 0.5441(3) 0.26076(15) 0.4649(2) 0.0291(8) Uani 1 1 d . . . C30 C 0.4278(3) 0.25783(16) 0.4432(2) 0.0292(8) Uani 1 1 d . . . C31 C 0.3766(3) 0.30864(16) 0.4100(2) 0.0396(10) Uani 1 1 d . . . H31A H 0.4176 0.3461 0.4034 0.047 Uiso 1 1 calc R . . C32 C 0.2660(3) 0.30487(18) 0.3866(3) 0.0508(12) Uani 1 1 d . . . H32A H 0.2319 0.3396 0.3629 0.061 Uiso 1 1 calc R . . C33 C 0.2049(3) 0.25126(18) 0.3972(2) 0.0447(11) Uani 1 1 d . . . H33A H 0.1285 0.2492 0.3817 0.054 Uiso 1 1 calc R . . C34 C 0.2549(3) 0.20038(17) 0.4307(2) 0.0370(9) Uani 1 1 d . . . H34A H 0.2130 0.1633 0.4378 0.044 Uiso 1 1 calc R . . C35 C 0.3653(3) 0.20333(16) 0.4537(2) 0.0317(9) Uani 1 1 d . . . H35A H 0.3992 0.1683 0.4768 0.038 Uiso 1 1 calc R . . C36 C 0.8228(3) 0.32014(15) 0.47467(19) 0.0268(8) Uani 1 1 d . . . C37 C 0.7679(3) 0.37485(15) 0.4573(2) 0.0316(9) Uani 1 1 d . . . H37A H 0.6881 0.3759 0.4567 0.038 Uiso 1 1 calc R . . C38 C 0.8277(3) 0.42817(16) 0.4407(2) 0.0410(10) Uani 1 1 d . . . H38A H 0.7888 0.4656 0.4293 0.049 Uiso 1 1 calc R . . C39 C 0.9434(3) 0.42717(18) 0.4406(2) 0.0426(10) Uani 1 1 d . . . H39A H 0.9844 0.4641 0.4303 0.051 Uiso 1 1 calc R . . C40 C 0.9997(3) 0.37249(18) 0.4556(2) 0.0412(10) Uani 1 1 d . . . H40A H 1.0794 0.3714 0.4548 0.049 Uiso 1 1 calc R . . C41 C 0.9398(3) 0.31917(17) 0.4719(2) 0.0333(9) Uani 1 1 d . . . H41A H 0.9789 0.2814 0.4813 0.040 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 Zn1 0.0206(2) 0.01895(19) 0.0248(2) 0.00065(16) -0.00202(16) -0.00052(15) Zn2 0.01956(19) 0.01959(19) 0.0232(2) -0.00005(16) 0.00037(16) -0.00021(15) Si1 0.0307(5) 0.0212(5) 0.0367(7) -0.0004(4) 0.0031(5) 0.0010(4) Si2 0.0424(6) 0.0223(5) 0.0589(9) -0.0013(5) -0.0269(6) -0.0003(5) Si3 0.0367(6) 0.0268(5) 0.0365(7) -0.0068(5) 0.0028(5) 0.0044(4) Si4 0.0297(5) 0.0227(5) 0.0441(7) 0.0037(5) 0.0024(5) -0.0036(4) O1 0.0243(12) 0.0231(11) 0.0203(14) 0.0034(10) -0.0044(10) -0.0038(9) N1 0.0199(14) 0.0250(14) 0.0259(18) -0.0013(13) -0.0043(13) -0.0005(12) N2 0.0219(14) 0.0224(14) 0.0200(17) -0.0009(12) -0.0015(12) 0.0023(11) N3 0.0189(14) 0.0218(14) 0.0268(19) 0.0014(12) 0.0005(13) -0.0005(11) C1 0.0245(19) 0.0301(19) 0.031(2) 0.0025(16) -0.0012(17) -0.0038(15) C2 0.0213(18) 0.038(2) 0.043(3) 0.0011(18) 0.0022(17) 0.0039(16) C3 0.0252(19) 0.0290(19) 0.055(3) 0.0039(18) -0.0006(19) 0.0063(16) C4 0.0257(18) 0.0287(19) 0.036(2) 0.0097(16) -0.0023(17) 0.0009(15) C5 0.0192(16) 0.0191(16) 0.030(2) 0.0001(15) -0.0076(15) -0.0042(14) C6 0.0256(18) 0.0251(17) 0.026(2) 0.0039(15) -0.0066(15) -0.0008(15) C7 0.0265(18) 0.0246(17) 0.024(2) -0.0017(15) 0.0004(16) -0.0029(15) C8 0.0277(18) 0.0188(16) 0.026(2) -0.0009(14) 0.0039(16) -0.0033(14) C9 0.034(2) 0.0212(17) 0.032(2) -0.0028(15) 0.0049(17) -0.0041(15) C10 0.0265(19) 0.0230(18) 0.047(3) -0.0047(17) 0.0103(18) 0.0045(15) C11 0.0196(18) 0.0274(18) 0.049(3) 0.0026(17) -0.0018(17) 0.0021(15) C12 0.0254(19) 0.0233(17) 0.033(2) -0.0003(15) -0.0005(17) -0.0019(15) C13 0.0291(18) 0.0199(16) 0.027(2) 0.0018(14) -0.0021(16) -0.0007(14) C14 0.058(3) 0.046(2) 0.049(3) -0.011(2) 0.016(2) -0.002(2) C15 0.030(2) 0.0307(19) 0.048(3) 0.0026(18) 0.0055(18) 0.0024(16) C16 0.031(2) 0.0282(19) 0.060(3) 0.0009(19) -0.002(2) 0.0037(16) C17 0.045(2) 0.034(2) 0.058(3) -0.004(2) -0.022(2) -0.0048(18) C18 0.152(5) 0.034(2) 0.079(4) 0.010(2) -0.079(4) -0.013(3) C19 0.028(2) 0.045(3) 0.143(6) -0.029(3) -0.022(3) 0.006(2) C20 0.0212(17) 0.0198(16) 0.031(2) 0.0011(15) -0.0036(15) 0.0023(14) C21 0.069(3) 0.046(2) 0.035(3) -0.007(2) -0.007(2) 0.000(2) C22 0.046(2) 0.052(3) 0.058(3) -0.005(2) 0.023(2) 0.007(2) C23 0.067(3) 0.037(2) 0.057(3) -0.012(2) 0.004(3) 0.016(2) C24 0.028(2) 0.036(2) 0.094(4) 0.013(2) 0.001(2) 0.0002(18) C25 0.083(3) 0.057(3) 0.050(3) -0.002(2) 0.028(3) -0.018(3) C26 0.045(2) 0.032(2) 0.078(4) 0.016(2) 0.003(2) -0.0052(19) C27 0.0296(19) 0.0287(18) 0.027(2) -0.0003(15) -0.0044(17) -0.0010(15) C28 0.036(2) 0.0285(19) 0.023(2) 0.0030(15) -0.0012(17) -0.0013(16) C29 0.030(2) 0.0279(19) 0.029(2) 0.0048(16) 0.0024(17) -0.0021(16) C30 0.0229(18) 0.036(2) 0.029(2) 0.0003(16) -0.0030(16) 0.0001(16) C31 0.039(2) 0.0243(19) 0.055(3) 0.0033(18) -0.006(2) -0.0040(17) C32 0.038(2) 0.039(2) 0.075(4) 0.008(2) -0.018(2) 0.0041(19) C33 0.027(2) 0.047(2) 0.060(3) -0.008(2) -0.012(2) 0.0033(19) C34 0.030(2) 0.039(2) 0.042(3) -0.0024(18) -0.0047(18) -0.0069(18) C35 0.032(2) 0.0293(19) 0.034(2) 0.0010(16) -0.0015(17) -0.0017(16) C36 0.0305(19) 0.0310(19) 0.019(2) 0.0020(15) -0.0012(15) -0.0050(15) C37 0.0296(19) 0.034(2) 0.031(2) 0.0040(17) -0.0016(17) -0.0015(16) C38 0.046(2) 0.028(2) 0.049(3) 0.0057(18) 0.000(2) -0.0015(18) C39 0.049(3) 0.042(2) 0.037(3) 0.0067(19) 0.006(2) -0.016(2) C40 0.029(2) 0.053(2) 0.042(3) 0.006(2) 0.0017(19) -0.0099(19) C41 0.031(2) 0.044(2) 0.026(2) 0.0057(17) -0.0009(17) -0.0007(17) _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 Zn1 C13 2.009(3) . ? Zn1 O1 2.022(2) . ? Zn1 N2 2.057(3) . ? Zn1 N1 2.189(3) . ? Zn1 Zn2 2.9637(5) . ? Zn2 C20 2.006(3) . ? Zn2 O1 2.011(2) . ? Zn2 N2 2.080(3) . ? Zn2 N3 2.123(3) . ? Si1 C13 1.844(3) . ? Si1 C15 1.872(4) . ? Si1 C14 1.875(4) . ? Si1 C16 1.879(3) . ? Si2 C13 1.850(3) . ? Si2 C18 1.872(5) . ? Si2 C17 1.878(4) . ? Si2 C19 1.885(5) . ? Si3 C20 1.835(4) . ? Si3 C21 1.869(4) . ? Si3 C22 1.876(4) . ? Si3 C23 1.886(4) . ? Si4 C20 1.851(3) . ? Si4 C25 1.866(5) . ? Si4 C24 1.870(4) . ? Si4 C26 1.884(4) . ? O1 C27 1.411(4) . ? N1 C5 1.341(4) . ? N1 C1 1.349(4) . ? N2 C7 1.456(4) . ? N2 C6 1.463(4) . ? N3 C8 1.337(4) . ? N3 C12 1.346(4) . ? C1 C2 1.372(5) . ? C1 H1A 0.9500 . ? C2 C3 1.380(5) . ? C2 H2A 0.9500 . ? C3 C4 1.378(5) . ? C3 H3A 0.9500 . ? C4 C5 1.388(4) . ? C4 H4A 0.9500 . ? C5 C6 1.498(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.507(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.393(5) . ? C9 C10 1.377(5) . ? C9 H9A 0.9500 . ? C10 C11 1.381(5) . ? C10 H10A 0.9500 . ? C11 C12 1.376(5) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.483(5) . ? C27 C36 1.521(4) . ? C27 H27A 1.0000 . ? C28 C29 1.196(5) . ? C29 C30 1.437(5) . ? C30 C31 1.385(5) . ? C30 C35 1.402(5) . ? C31 C32 1.382(5) . ? C31 H31A 0.9500 . ? C32 C33 1.377(5) . ? C32 H32A 0.9500 . ? C33 C34 1.382(5) . ? C33 H33A 0.9500 . ? C34 C35 1.376(5) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.381(5) . ? C36 C41 1.393(5) . ? C37 C38 1.384(5) . ? C37 H37A 0.9500 . ? C38 C39 1.378(5) . ? C38 H38A 0.9500 . ? C39 C40 1.379(5) . ? C39 H39A 0.9500 . ? C40 C41 1.383(5) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Zn1 O1 124.93(12) . . ? C13 Zn1 N2 135.61(13) . . ? O1 Zn1 N2 87.08(9) . . ? C13 Zn1 N1 121.41(11) . . ? O1 Zn1 N1 94.34(9) . . ? N2 Zn1 N1 79.77(10) . . ? C13 Zn1 Zn2 153.45(9) . . ? O1 Zn1 Zn2 42.55(6) . . ? N2 Zn1 Zn2 44.56(7) . . ? N1 Zn1 Zn2 85.04(7) . . ? C20 Zn2 O1 129.02(12) . . ? C20 Zn2 N2 123.86(12) . . ? O1 Zn2 N2 86.76(10) . . ? C20 Zn2 N3 124.40(11) . . ? O1 Zn2 N3 97.65(9) . . ? N2 Zn2 N3 80.87(10) . . ? C20 Zn2 Zn1 143.65(9) . . ? O1 Zn2 Zn1 42.85(6) . . ? N2 Zn2 Zn1 43.93(7) . . ? N3 Zn2 Zn1 90.21(7) . . ? C13 Si1 C15 114.11(16) . . ? C13 Si1 C14 110.81(18) . . ? C15 Si1 C14 107.39(19) . . ? C13 Si1 C16 112.02(16) . . ? C15 Si1 C16 104.99(17) . . ? C14 Si1 C16 107.08(18) . . ? C13 Si2 C18 111.5(2) . . ? C13 Si2 C17 116.98(16) . . ? C18 Si2 C17 104.6(2) . . ? C13 Si2 C19 109.05(19) . . ? C18 Si2 C19 109.1(3) . . ? C17 Si2 C19 105.15(19) . . ? C20 Si3 C21 111.26(17) . . ? C20 Si3 C22 109.36(18) . . ? C21 Si3 C22 109.7(2) . . ? C20 Si3 C23 114.80(18) . . ? C21 Si3 C23 106.16(19) . . ? C22 Si3 C23 105.29(19) . . ? C20 Si4 C25 111.01(18) . . ? C20 Si4 C24 112.39(18) . . ? C25 Si4 C24 107.5(2) . . ? C20 Si4 C26 113.43(16) . . ? C25 Si4 C26 105.7(2) . . ? C24 Si4 C26 106.43(18) . . ? C27 O1 Zn2 131.57(18) . . ? C27 O1 Zn1 133.73(18) . . ? Zn2 O1 Zn1 94.60(9) . . ? C5 N1 C1 118.3(3) . . ? C5 N1 Zn1 110.9(2) . . ? C1 N1 Zn1 130.8(2) . . ? C7 N2 C6 107.9(3) . . ? C7 N2 Zn1 122.56(19) . . ? C6 N2 Zn1 110.09(19) . . ? C7 N2 Zn2 108.07(18) . . ? C6 N2 Zn2 116.35(19) . . ? Zn1 N2 Zn2 91.51(11) . . ? C8 N3 C12 119.4(3) . . ? C8 N3 Zn2 112.1(2) . . ? C12 N3 Zn2 128.4(2) . . ? N1 C1 C2 123.2(3) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C1 C2 C3 118.4(3) . . ? C1 C2 H2A 120.8 . . ? C3 C2 H2A 120.8 . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 117.5(3) . . ? C4 C5 C6 121.0(3) . . ? N2 C6 C5 112.1(3) . . ? N2 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 112.1(3) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N3 C8 C9 120.8(3) . . ? N3 C8 C7 116.8(3) . . ? C9 C8 C7 122.3(3) . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C9 C10 C11 118.9(3) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C12 C11 C10 119.0(3) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? N3 C12 C11 122.1(3) . . ? N3 C12 H12A 118.9 . . ? C11 C12 H12A 118.9 . . ? Si1 C13 Si2 118.12(18) . . ? Si1 C13 Zn1 112.28(16) . . ? Si2 C13 Zn1 109.50(15) . . ? Si1 C13 H13A 105.3 . . ? Si2 C13 H13A 105.3 . . ? Zn1 C13 H13A 105.3 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 Si4 120.34(17) . . ? Si3 C20 Zn2 111.64(17) . . ? Si4 C20 Zn2 111.79(16) . . ? Si3 C20 H20A 103.6 . . ? Si4 C20 H20A 103.6 . . ? Zn2 C20 H20A 103.6 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C27 C28 111.1(3) . . ? O1 C27 C36 110.7(3) . . ? C28 C27 C36 112.1(3) . . ? O1 C27 H27A 107.6 . . ? C28 C27 H27A 107.6 . . ? C36 C27 H27A 107.6 . . ? C29 C28 C27 177.1(4) . . ? C28 C29 C30 178.4(4) . . ? C31 C30 C35 119.0(3) . . ? C31 C30 C29 120.2(3) . . ? C35 C30 C29 120.7(3) . . ? C30 C31 C32 120.1(3) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C33 C32 C31 120.6(4) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C34 119.8(3) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? C35 C34 C33 120.2(3) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C30 120.3(3) . . ? C34 C35 H35A 119.9 . . ? C30 C35 H35A 119.9 . . ? C37 C36 C41 118.4(3) . . ? C37 C36 C27 123.6(3) . . ? C41 C36 C27 117.9(3) . . ? C36 C37 C38 120.8(3) . . ? C36 C37 H37A 119.6 . . ? C38 C37 H37A 119.6 . . ? C39 C38 C37 120.2(3) . . ? C39 C38 H38A 119.9 . . ? C37 C38 H38A 119.9 . . ? C38 C39 C40 119.8(3) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C39 C40 C41 119.9(3) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C40 C41 C36 120.8(3) . . ? C40 C41 H41A 119.6 . . ? C36 C41 H41A 119.6 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.469 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.087