Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Akihiko Ishii' 'Aki Furukawa' 'Juzo Nakayama' 'Hideaki Oshida' 'Takeshi Takahashi' 'Akira Tawata' _publ_contact_author_name 'Prof Akihiko Ishii' _publ_contact_author_address ; Prof Akihiko Ishii Department of Chemistry, Faculty of Science Saitama University Shimo-okubo 255 Saitama 338-8570 JAPAN ; _publ_contact_author_email 'ishiiaki@chem.saitama-u.ac.jp' _publ_contact_author_fax '+81-48-858-3700' _publ_contact_author_phone '+81-48-858-3394' _publ_requested_journal 'Chemical Communications' _publ_section_title ; First Synthesis and Characterization of Isolable Thioselenenic acid, Triptycene-9-thioselenenic Acid ; _publ_section_abstract ; We present the crystal and molecular structure of Triptycene-9-thioselenenic acid ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. All diagrams and calculations were performed using maXus (Bruker Nonius, Delft & MacScience, Japan). ; _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Sheldrick, G.M. (1997). SHELXS-97. Program for Crystal Structure Solution. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXL97. Program for the Refinement of Crystal Structures. University of Gottingen, Germany. Blessing, R.H. (1995), Acta. Cryst. A51, 33-38. ; data_1 _database_code_CSD 191691 _audit_creation_method 'maXus' _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Plates' _exptl_crystal_colour 'Pale yellow' _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment 'refxyz' # Submission details _publ_requested_journal 'Chemical Communications' _diffrn_measurement_device 'Mac Science MXC3KHF' _diffrn_measurement_method '¥q ¥w scans' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'maXus (Mackay et al., 1999)' _cell_measurement_reflns_used 22 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _diffrn_radiation_source 'fine-focus sealed tube' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 -4 4 3 1 4 6 -1 5 _diffrn_standards_decay_% 3.873 _diffrn_standards_interval_time 1918 _diffrn_standards_number 3 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 loop_ _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type 'X=UH' _diffrn_orient_matrix_UB_11 0.13533 _diffrn_orient_matrix_UB_12 -0.02770 _diffrn_orient_matrix_UB_13 -0.01813 _diffrn_orient_matrix_UB_21 0.00334 _diffrn_orient_matrix_UB_22 0.02878 _diffrn_orient_matrix_UB_23 -0.07654 _diffrn_orient_matrix_UB_31 -0.02237 _diffrn_orient_matrix_UB_32 0.12522 _diffrn_orient_matrix_UB_33 0.01198 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 365.356 _diffrn_radiation_type ' CuK¥a' loop_ _symmetry_equiv_pos_as_xyz '+X,+Y,+Z' '-X,-Y,-Z' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' _chemical_formula_moiety 'C20 H14 S Se ' _chemical_formula_sum 'C20 H14 S Se ' _chemical_name_systematic ; Triptycene-9-thioselenenic acid ; _cell_length_a 8.181(2) _cell_length_b 8.217(1) _cell_length_c 13.175(3) _cell_angle_alpha 82.53(1) _cell_angle_beta 72.58(1) _cell_angle_gamma 67.82(1) _cell_volume 782.4(2) _diffrn_reflns_number 3166 _diffrn_reflns_theta_max 70.00 _diffrn_reflns_av_R_equivalents 0.014 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; psi-scan (North, Philips & Mathews, 1968) ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _exptl_absorpt_coefficient_mu 4.417 _reflns_number_total 2944 _reflns_number_gt 2822 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0514P)^2^+0.4892P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0069(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^¥l^3^/sin(2¥q)]^-1/4^' _refine_ls_number_reflns 2944 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.74384(3) 0.07101(3) 0.13932(2) 0.04449(13) Uani 1 1 d . . . S1 S 0.76162(10) -0.01710(12) -0.01400(6) 0.0624(2) Uani 1 1 d . . . C1 C 0.4848(3) 0.1205(3) 0.22014(17) 0.0351(4) Uani 1 1 d . . . C3 C 0.3752(3) 0.3627(3) 0.07998(19) 0.0405(5) Uani 1 1 d . . . C2 C 0.3434(3) 0.2676(3) 0.17303(17) 0.0345(4) Uani 1 1 d . . . C13 C 0.5224(4) -0.2080(3) 0.2064(2) 0.0454(5) Uani 1 1 d . . . C7 C 0.1640(3) 0.3044(3) 0.23738(19) 0.0410(5) Uani 1 1 d . . . C9 C 0.2413(3) 0.0044(3) 0.3032(2) 0.0437(5) Uani 1 1 d . . . C14 C 0.4216(3) -0.0376(3) 0.24051(17) 0.0372(5) Uani 1 1 d . . . C4 C 0.2288(4) 0.4931(3) 0.0506(2) 0.0500(6) Uani 1 1 d . . . C8 C 0.1509(4) 0.1940(3) 0.3386(2) 0.0465(6) Uani 1 1 d . . . C15 C 0.4564(4) 0.1831(3) 0.33127(18) 0.0417(5) Uani 1 1 d . . . C20 C 0.2761(4) 0.2236(3) 0.39411(19) 0.0469(6) Uani 1 1 d . . . C10 C 0.1604(5) -0.1218(4) 0.3289(3) 0.0572(7) Uani 1 1 d . . . C12 C 0.4407(5) -0.3340(3) 0.2327(2) 0.0555(7) Uani 1 1 d . . . C16 C 0.5867(5) 0.2020(4) 0.3712(2) 0.0563(7) Uani 1 1 d . . . C19 C 0.2264(6) 0.2836(4) 0.4959(2) 0.0659(9) Uani 1 1 d . . . C5 C 0.0533(4) 0.5284(4) 0.1136(3) 0.0581(7) Uani 1 1 d . . . C6 C 0.0189(4) 0.4335(4) 0.2074(3) 0.0531(6) Uani 1 1 d . . . C11 C 0.2630(5) -0.2925(4) 0.2930(3) 0.0626(8) Uani 1 1 d . . . C17 C 0.5344(7) 0.2612(5) 0.4745(3) 0.0783(11) Uani 1 1 d . . . C18 C 0.3585(7) 0.3013(5) 0.5350(3) 0.0816(12) Uani 1 1 d . . . H1 H 0.743(9) 0.128(9) -0.061(5) 0.17(2) Uiso 1 1 d . . . H3 H 0.490(4) 0.334(4) 0.038(2) 0.046(7) Uiso 1 1 d . . . H13 H 0.637(5) -0.236(4) 0.169(3) 0.061(9) Uiso 1 1 d . . . H4 H 0.252(4) 0.554(4) -0.011(3) 0.057(8) Uiso 1 1 d . . . H8 H 0.032(4) 0.218(4) 0.380(2) 0.047(7) Uiso 1 1 d . . . H10 H 0.055(5) -0.095(4) 0.365(3) 0.054(9) Uiso 1 1 d . . . H12 H 0.513(5) -0.445(5) 0.210(3) 0.076(11) Uiso 1 1 d . . . H16 H 0.706(4) 0.177(4) 0.328(2) 0.045(7) Uiso 1 1 d . . . H19 H 0.113(6) 0.311(5) 0.530(3) 0.079(12) Uiso 1 1 d . . . H5 H -0.048(5) 0.620(5) 0.095(3) 0.080(11) Uiso 1 1 d . . . H6 H -0.088(5) 0.444(4) 0.248(3) 0.064(9) Uiso 1 1 d . . . H11 H 0.197(6) -0.379(6) 0.309(4) 0.100(14) Uiso 1 1 d . . . H17 H 0.617(6) 0.269(5) 0.498(3) 0.079(12) Uiso 1 1 d . . . H18 H 0.330(6) 0.334(6) 0.599(4) 0.095(13) 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 Se1 0.03382(17) 0.04863(19) 0.04937(19) -0.00171(11) -0.01138(11) -0.01267(12) S1 0.0541(4) 0.0752(5) 0.0519(4) -0.0167(3) -0.0055(3) -0.0183(3) C1 0.0342(10) 0.0324(10) 0.0373(11) -0.0007(8) -0.0085(8) -0.0112(8) C3 0.0420(13) 0.0367(11) 0.0418(12) -0.0001(9) -0.0101(10) -0.0140(10) C2 0.0356(11) 0.0292(10) 0.0385(11) -0.0027(8) -0.0106(9) -0.0103(8) C13 0.0518(15) 0.0353(12) 0.0453(13) -0.0024(10) -0.0131(11) -0.0110(10) C7 0.0368(12) 0.0367(11) 0.0457(12) -0.0053(9) -0.0065(10) -0.0111(9) C9 0.0467(13) 0.0392(12) 0.0444(12) 0.0002(10) -0.0076(10) -0.0185(10) C14 0.0443(12) 0.0322(10) 0.0371(11) 0.0007(8) -0.0128(9) -0.0149(9) C4 0.0567(15) 0.0429(13) 0.0502(14) 0.0081(11) -0.0226(12) -0.0143(11) C8 0.0425(13) 0.0407(12) 0.0459(13) -0.0034(10) 0.0036(11) -0.0149(10) C15 0.0558(14) 0.0324(11) 0.0390(11) 0.0028(9) -0.0180(10) -0.0153(10) C20 0.0653(16) 0.0346(11) 0.0367(12) -0.0002(9) -0.0076(11) -0.0181(11) C10 0.0586(18) 0.0528(15) 0.0610(17) 0.0011(13) -0.0032(14) -0.0316(14) C12 0.077(2) 0.0343(13) 0.0574(16) -0.0023(11) -0.0209(14) -0.0202(13) C16 0.070(2) 0.0499(15) 0.0571(16) -0.0001(12) -0.0319(15) -0.0191(14) C19 0.090(3) 0.0498(16) 0.0416(14) -0.0031(12) -0.0005(16) -0.0206(16) C5 0.0469(15) 0.0479(14) 0.0706(18) 0.0030(13) -0.0242(13) -0.0024(12) C6 0.0353(13) 0.0492(14) 0.0654(17) -0.0086(12) -0.0089(12) -0.0061(11) C11 0.082(2) 0.0485(15) 0.0688(18) 0.0051(13) -0.0190(16) -0.0385(15) C17 0.109(3) 0.069(2) 0.071(2) -0.0091(17) -0.053(2) -0.024(2) C18 0.131(4) 0.069(2) 0.0458(17) -0.0116(15) -0.032(2) -0.026(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 Se1 C1 1.975(2) . ? Se1 S1 2.1796(9) . ? C1 C14 1.536(3) . ? C1 C2 1.537(3) . ? C1 C15 1.538(3) . ? C3 C2 1.377(3) . ? C3 C4 1.390(4) . ? C2 C7 1.397(3) . ? C13 C14 1.383(3) . ? C13 C12 1.389(4) . ? C7 C6 1.383(4) . ? C7 C8 1.512(3) . ? C9 C10 1.386(4) . ? C9 C14 1.392(3) . ? C9 C8 1.518(3) . ? C4 C5 1.367(4) . ? C8 C20 1.525(4) . ? C15 C16 1.385(4) . ? C15 C20 1.394(4) . ? C20 C19 1.379(4) . ? C10 C11 1.394(4) . ? C12 C11 1.365(5) . ? C16 C17 1.393(5) . ? C19 C18 1.387(6) . ? C5 C6 1.386(4) . ? C17 C18 1.356(6) . ? S1 H1 1.24(6) . ? C3 H3 0.90(3) . ? C13 H13 0.87(3) . ? C4 H4 0.90(3) . ? C8 H8 0.92(3) . ? C10 H10 0.81(3) . ? C12 H12 0.91(4) . ? C16 H16 0.93(3) . ? C19 H19 0.85(4) . ? C5 H5 0.96(4) . ? C6 H6 0.86(4) . ? C11 H11 1.01(4) . ? C17 H17 0.84(4) . ? C18 H18 0.85(5) . ? 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 Se1 S1 103.85(7) . . ? C14 C1 C2 106.19(17) . . ? C14 C1 C15 105.15(17) . . ? C2 C1 C15 105.31(17) . . ? C14 C1 Se1 115.62(15) . . ? C2 C1 Se1 115.27(15) . . ? C15 C1 Se1 108.37(15) . . ? C2 C3 C4 119.8(2) . . ? C3 C2 C7 119.4(2) . . ? C3 C2 C1 128.0(2) . . ? C7 C2 C1 112.54(19) . . ? C14 C13 C12 119.5(3) . . ? C6 C7 C2 120.4(2) . . ? C6 C7 C8 126.0(2) . . ? C2 C7 C8 113.5(2) . . ? C10 C9 C14 120.5(2) . . ? C10 C9 C8 125.7(2) . . ? C14 C9 C8 113.7(2) . . ? C13 C14 C9 119.6(2) . . ? C13 C14 C1 127.9(2) . . ? C9 C14 C1 112.48(19) . . ? C5 C4 C3 120.6(3) . . ? C7 C8 C9 105.6(2) . . ? C7 C8 C20 105.8(2) . . ? C9 C8 C20 106.0(2) . . ? C16 C15 C20 120.1(2) . . ? C16 C15 C1 127.3(2) . . ? C20 C15 C1 112.6(2) . . ? C19 C20 C15 120.2(3) . . ? C19 C20 C8 126.5(3) . . ? C15 C20 C8 113.4(2) . . ? C9 C10 C11 119.1(3) . . ? C11 C12 C13 120.9(3) . . ? C15 C16 C17 119.0(3) . . ? C20 C19 C18 119.2(4) . . ? C4 C5 C6 120.3(2) . . ? C7 C6 C5 119.4(3) . . ? C12 C11 C10 120.2(3) . . ? C18 C17 C16 120.7(4) . . ? C17 C18 C19 121.0(3) . . ? Se1 S1 H1 96(3) . . ? C2 C3 H3 118.5(18) . . ? C4 C3 H3 121.6(18) . . ? C14 C13 H13 120(2) . . ? C12 C13 H13 120(2) . . ? C5 C4 H4 120(2) . . ? C3 C4 H4 119(2) . . ? C7 C8 H8 113.3(18) . . ? C9 C8 H8 112.0(18) . . ? C20 C8 H8 113.5(18) . . ? C9 C10 H10 119(2) . . ? C11 C10 H10 122(2) . . ? C11 C12 H12 123(2) . . ? C13 C12 H12 116(2) . . ? C15 C16 H16 118.8(18) . . ? C17 C16 H16 122.2(18) . . ? C20 C19 H19 116(3) . . ? C18 C19 H19 124(3) . . ? C4 C5 H5 121(2) . . ? C6 C5 H5 119(2) . . ? C7 C6 H6 115(2) . . ? C5 C6 H6 125(2) . . ? C12 C11 H11 123(3) . . ? C10 C11 H11 117(3) . . ? C18 C17 H17 122(3) . . ? C16 C17 H17 117(3) . . ? C17 C18 H18 119(3) . . ? C19 C18 H18 120(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 70.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.454 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.057 #===END data_Compound_7 _database_code_CSD 191692 _audit_creation_method 'maXus' _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Cube' _exptl_crystal_colour 'Yellow' _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment 'refxyz' # Submission details _publ_requested_journal 'Chemical Communications' _diffrn_measurement_device 'DIP Image plate' _computing_data_collection 'DIP Image plate' _computing_data_reduction 'maXus (Mackay et al., 1999)' _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 714.356 _diffrn_radiation_type ' MoK¥a' loop_ _symmetry_equiv_pos_as_xyz '+X,+Y,+Z' '-X+ 1/2,-Y,+Z+ 1/2' '+X+ 1/2,-Y+ 1/2,-Z' '-X,+Y+ 1/2,-Z+ 1/2' _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_cell_setting 'Orthorhombic' _chemical_formula_moiety 'C38 H28 S Se Sn ' _chemical_formula_sum 'C38 H28 S Se Sn ' _chemical_name_systematic ; Trip-Se-S-SnPh3 (Trip = 9-triptycyl) ; _cell_length_a 11.4730(4) _cell_length_b 15.4100(6) _cell_length_c 17.6340(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3117.7(2) _diffrn_reflns_number 20437 _diffrn_reflns_theta_max 27.08 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_full 27.08 _diffrn_measurement_method 'IP' _computing_cell_refinement 'HKL Scalepack' _computing_structure_solution 'DIRDIF (Buerskens et al., 1992)' _atom_sites_solution_primary vecmap _atom_sites_solution_secondary difmap # Absorption correction _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 0.785 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_reflns_av_R_equivalents 0.054 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _exptl_absorpt_coefficient_mu 2.079 _reflns_number_total 6631 _reflns_number_gt 4849 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0347P)^2^+2.5037P] where P=(Fo^2^+2Fc^2^)/3' _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 0.084(14) _refine_ls_number_reflns 6631 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Sn1 Sn 0.20904(4) 0.02401(3) 0.03116(2) 0.05358(13) Uani 1 1 d . . . Se1 Se -0.06490(6) 0.04990(4) 0.11492(3) 0.05240(17) Uani 1 1 d . . . S1 S 0.01886(13) -0.04517(11) 0.03796(9) 0.0573(4) Uani 1 1 d . . . C9 C 0.0600(5) -0.0908(4) 0.2282(3) 0.0491(14) Uani 1 1 d . . . C8 C -0.0578(5) -0.0878(3) 0.2333(3) 0.0425(13) Uani 1 1 d . . . C14 C -0.2022(5) 0.0277(4) 0.2494(3) 0.0419(12) Uani 1 1 d . . . C15 C -0.2074(6) 0.1159(4) 0.2544(3) 0.0498(14) Uani 1 1 d . . . C5 C -0.4201(7) -0.1901(5) 0.1141(5) 0.075(2) Uani 1 1 d . . . C4 C -0.3840(6) -0.1887(4) 0.1884(5) 0.068(2) Uani 1 1 d . . . C13 C -0.1163(5) -0.1376(4) 0.2868(3) 0.0486(15) Uani 1 1 d . . . C1 C -0.1407(5) -0.0276(4) 0.1889(3) 0.0417(12) Uani 1 1 d . . . C23 C 0.3704(7) -0.2077(4) -0.0646(4) 0.0652(19) Uani 1 1 d . . . C31 C 0.2970(7) 0.1074(5) 0.2631(4) 0.073(2) Uani 1 1 d . . . C7 C -0.2760(6) -0.0852(4) 0.0802(3) 0.0553(16) Uani 1 1 d . . . C19 C -0.2575(5) -0.0239(4) 0.3034(3) 0.0482(14) Uani 1 1 d . . . C20 C -0.2455(5) -0.1214(4) 0.2879(4) 0.0533(17) Uani 1 1 d . . . C2 C -0.2370(5) -0.0837(4) 0.1545(3) 0.0465(15) Uani 1 1 d . . . C32 C 0.2441(6) 0.0978(5) 0.1938(4) 0.0631(18) Uani 1 1 d . . . C12 C -0.0555(7) -0.1903(4) 0.3351(3) 0.0597(18) Uani 1 1 d . . . C33 C 0.1770(6) 0.1475(5) -0.0184(4) 0.0666(19) Uani 1 1 d . . . C16 C -0.2662(6) 0.1535(4) 0.3146(4) 0.0621(19) Uani 1 1 d . . . C26 C 0.3934(6) -0.0337(5) -0.0831(4) 0.0653(18) Uani 1 1 d . . . C3 C -0.2922(6) -0.1348(4) 0.2084(3) 0.0521(14) Uani 1 1 d . . . C21 C 0.3099(5) -0.0638(4) -0.0333(3) 0.0536(14) Uani 1 1 d . . . C27 C 0.2864(6) 0.0426(4) 0.1390(3) 0.0554(15) Uani 1 1 d . . . C18 C -0.3148(5) 0.0133(5) 0.3640(3) 0.0568(16) Uani 1 1 d . . . C24 C 0.4519(7) -0.1769(5) -0.1138(4) 0.073(2) Uani 1 1 d . . . C11 C 0.0649(7) -0.1942(4) 0.3301(4) 0.0637(19) Uani 1 1 d . . . C10 C 0.1214(6) -0.1439(4) 0.2767(4) 0.0592(18) Uani 1 1 d . . . C6 C -0.3682(7) -0.1383(5) 0.0607(4) 0.070(2) Uani 1 1 d . . . C36 C 0.1375(13) 0.3125(8) -0.0750(8) 0.130(5) Uani 1 1 d . . . C30 C 0.3933(7) 0.0635(7) 0.2792(5) 0.098(3) Uani 1 1 d . . . C17 C -0.3170(6) 0.1039(5) 0.3686(4) 0.0636(18) Uani 1 1 d . . . C22 C 0.3009(6) -0.1530(4) -0.0244(4) 0.0639(17) Uani 1 1 d . . . C25 C 0.4633(7) -0.0891(6) -0.1225(4) 0.080(2) Uani 1 1 d . . . C35 C 0.2181(12) 0.2998(6) -0.0235(6) 0.115(4) Uani 1 1 d . . . C29 C 0.4397(9) 0.0112(8) 0.2260(6) 0.135(5) Uani 1 1 d . . . C28 C 0.3862(7) -0.0020(6) 0.1560(5) 0.097(3) Uani 1 1 d . . . C34 C 0.2387(8) 0.2184(5) 0.0049(5) 0.090(3) Uani 1 1 d . . . C37 C 0.0757(12) 0.2444(8) -0.1012(8) 0.141(5) Uani 1 1 d . . . C38 C 0.0953(9) 0.1614(7) -0.0714(6) 0.119(4) Uani 1 1 d . . . H9 H 0.0986 -0.0556 0.1910 0.059 Uiso 1 1 d R . . H15 H -0.1687 0.1506 0.2169 0.060 Uiso 1 1 d R . . H5 H -0.4817 -0.2286 0.0990 0.090 Uiso 1 1 d R . . H4 H -0.4216 -0.2247 0.2255 0.081 Uiso 1 1 d R . . H23 H 0.3596 -0.2691 -0.0582 0.078 Uiso 1 1 d R . . H31 H 0.2633 0.1448 0.3007 0.087 Uiso 1 1 d R . . H7 H -0.2390 -0.0499 0.0423 0.066 Uiso 1 1 d R . . H20 H -0.2860 -0.1542 0.3259 0.064 Uiso 1 1 d R . . H32 H 0.1753 0.1306 0.1821 0.076 Uiso 1 1 d R . . H12 H -0.0963 -0.2252 0.3716 0.072 Uiso 1 1 d R . . H16 H -0.2730 0.2154 0.3181 0.075 Uiso 1 1 d R . . H26 H 0.4035 0.0279 -0.0880 0.078 Uiso 1 1 d R . . H18 H -0.3490 -0.0239 0.4017 0.068 Uiso 1 1 d R . . H24 H 0.5015 -0.2170 -0.1402 0.087 Uiso 1 1 d R . . H11 H 0.1075 -0.2311 0.3641 0.076 Uiso 1 1 d R . . H10 H 0.2048 -0.1462 0.2729 0.071 Uiso 1 1 d R . . H6 H -0.3955 -0.1375 0.0093 0.084 Uiso 1 1 d R . . H36 H 0.1259 0.3696 -0.0955 0.156 Uiso 1 1 d R . . H30 H 0.4301 0.0697 0.3278 0.118 Uiso 1 1 d R . . H17 H -0.3557 0.1316 0.4104 0.076 Uiso 1 1 d R . . H22 H 0.2449 -0.1762 0.0106 0.077 Uiso 1 1 d R . . H25 H 0.5192 -0.0675 -0.1584 0.096 Uiso 1 1 d R . . H35 H 0.2618 0.3479 -0.0039 0.138 Uiso 1 1 d R . . H29 H 0.5102 -0.0199 0.2367 0.161 Uiso 1 1 d R . . H28 H 0.4211 -0.0375 0.1175 0.116 Uiso 1 1 d R . . H34 H 0.2982 0.2102 0.0425 0.108 Uiso 1 1 d R . . H37 H 0.0178 0.2537 -0.1396 0.169 Uiso 1 1 d R . . H38 H 0.0497 0.1131 -0.0888 0.143 Uiso 1 1 d 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 Sn1 0.0490(2) 0.0561(2) 0.0556(2) -0.0049(2) 0.0074(2) -0.0004(2) Se1 0.0516(4) 0.0499(3) 0.0557(4) 0.0104(3) 0.0071(3) 0.0035(3) S1 0.0513(9) 0.0676(10) 0.0529(8) -0.0065(9) 0.0056(7) -0.0078(7) C9 0.046(4) 0.047(3) 0.054(4) -0.001(3) -0.002(3) 0.002(3) C8 0.043(4) 0.037(3) 0.047(3) -0.001(3) -0.006(3) 0.000(3) C14 0.029(3) 0.051(3) 0.045(3) -0.001(3) 0.001(2) 0.005(3) C15 0.051(4) 0.041(3) 0.057(4) 0.001(3) 0.000(3) 0.010(3) C5 0.047(4) 0.077(5) 0.102(6) -0.023(5) -0.014(5) -0.001(4) C4 0.045(4) 0.059(4) 0.099(6) -0.005(4) -0.002(4) 0.000(3) C13 0.049(4) 0.043(3) 0.054(4) 0.001(3) -0.003(3) -0.006(3) C1 0.037(3) 0.044(3) 0.045(3) 0.000(3) -0.001(2) 0.003(3) C23 0.065(5) 0.053(4) 0.077(5) -0.011(4) -0.003(4) -0.004(4) C31 0.061(5) 0.078(5) 0.080(5) -0.029(4) 0.002(4) -0.009(5) C7 0.045(4) 0.068(4) 0.052(3) -0.009(3) -0.007(3) 0.016(3) C19 0.036(3) 0.056(3) 0.053(3) 0.002(3) -0.004(2) 0.002(3) C20 0.054(4) 0.052(4) 0.054(4) 0.007(3) 0.003(3) -0.005(3) C2 0.044(4) 0.047(3) 0.049(3) 0.002(3) -0.002(3) 0.005(3) C32 0.047(4) 0.064(4) 0.078(5) -0.012(4) 0.007(3) 0.002(3) C12 0.088(6) 0.046(4) 0.045(3) 0.007(3) 0.002(4) 0.003(4) C33 0.059(5) 0.066(4) 0.075(5) 0.006(4) 0.021(4) -0.005(3) C16 0.065(5) 0.050(4) 0.071(4) -0.008(3) 0.000(4) 0.014(3) C26 0.060(4) 0.067(4) 0.069(4) 0.015(4) 0.022(3) 0.004(4) C3 0.042(3) 0.054(3) 0.061(4) -0.004(3) -0.004(3) 0.008(3) C21 0.048(4) 0.059(4) 0.054(3) -0.005(3) 0.008(3) -0.003(3) C27 0.040(3) 0.060(4) 0.066(4) -0.020(3) 0.000(3) -0.001(3) C18 0.046(4) 0.075(4) 0.049(3) 0.006(3) 0.000(3) 0.000(3) C24 0.072(5) 0.079(5) 0.068(5) -0.017(4) 0.004(4) 0.022(4) C11 0.081(6) 0.057(4) 0.053(4) -0.008(3) -0.018(4) 0.030(4) C10 0.053(4) 0.066(4) 0.059(4) -0.012(4) -0.017(3) 0.016(3) C6 0.057(5) 0.089(5) 0.065(4) -0.023(4) -0.022(4) 0.015(4) C36 0.152(13) 0.089(8) 0.149(12) 0.047(8) 0.056(10) 0.028(9) C30 0.066(6) 0.143(9) 0.085(6) -0.037(6) -0.031(5) 0.020(6) C17 0.063(5) 0.071(5) 0.057(4) -0.012(4) 0.008(3) 0.007(4) C22 0.069(4) 0.053(4) 0.070(4) 0.001(3) 0.011(4) -0.013(4) C25 0.067(5) 0.101(6) 0.071(5) 0.012(5) 0.030(4) 0.007(5) C35 0.175(12) 0.069(6) 0.102(7) 0.010(6) 0.070(8) -0.022(7) C29 0.086(6) 0.188(12) 0.130(8) -0.063(8) -0.057(6) 0.070(8) C28 0.072(6) 0.114(8) 0.105(6) -0.051(5) -0.028(5) 0.034(5) C34 0.116(8) 0.078(6) 0.077(5) -0.003(4) 0.034(5) -0.016(5) C37 0.114(9) 0.128(10) 0.181(12) 0.064(10) -0.025(9) 0.007(8) C38 0.107(8) 0.103(7) 0.148(10) 0.041(7) -0.031(7) -0.012(6) _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 Sn1 C21 2.112(6) . ? Sn1 C27 2.118(6) . ? Sn1 C33 2.126(7) . ? Sn1 S1 2.4314(16) . ? Se1 C1 1.971(5) . ? Se1 S1 2.2162(17) . ? C9 C8 1.355(8) . ? C9 C10 1.377(8) . ? C8 C13 1.389(8) . ? C8 C1 1.542(7) . ? C14 C15 1.364(8) . ? C14 C19 1.393(8) . ? C14 C1 1.536(7) . ? C15 C16 1.383(9) . ? C5 C6 1.370(11) . ? C5 C4 1.376(10) . ? C4 C3 1.387(9) . ? C13 C12 1.368(9) . ? C13 C20 1.503(9) . ? C1 C2 1.528(8) . ? C23 C22 1.360(9) . ? C23 C24 1.361(10) . ? C31 C30 1.326(11) . ? C31 C32 1.372(10) . ? C7 C6 1.380(9) . ? C7 C2 1.386(8) . ? C19 C18 1.380(8) . ? C19 C20 1.534(9) . ? C20 C3 1.516(9) . ? C2 C3 1.387(8) . ? C32 C27 1.376(8) . ? C12 C11 1.386(11) . ? C33 C38 1.341(11) . ? C33 C34 1.365(10) . ? C16 C17 1.354(10) . ? C26 C25 1.362(10) . ? C26 C21 1.379(8) . ? C21 C22 1.388(8) . ? C27 C28 1.369(9) . ? C18 C17 1.399(10) . ? C24 C25 1.369(10) . ? C11 C10 1.381(10) . ? C36 C35 1.310(16) . ? C36 C37 1.348(17) . ? C30 C29 1.346(12) . ? C35 C34 1.371(12) . ? C29 C28 1.392(11) . ? C37 C38 1.401(14) . ? C9 H9 0.9600 . ? C15 H15 0.9599 . ? C5 H5 0.9602 . ? C4 H4 0.9599 . ? C23 H23 0.9600 . ? C31 H31 0.9598 . ? C7 H7 0.9601 . ? C20 H20 0.9599 . ? C32 H32 0.9601 . ? C12 H12 0.9599 . ? C16 H16 0.9600 . ? C26 H26 0.9601 . ? C18 H18 0.9603 . ? C24 H24 0.9600 . ? C11 H11 0.9599 . ? C10 H10 0.9600 . ? C6 H6 0.9600 . ? C36 H36 0.9599 . ? C30 H30 0.9599 . ? C17 H17 0.9600 . ? C22 H22 0.9601 . ? C25 H25 0.9600 . ? C35 H35 0.9599 . ? C29 H29 0.9600 . ? C28 H28 0.9599 . ? C34 H34 0.9601 . ? C37 H37 0.9599 . ? C38 H38 0.9599 . ? 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 Sn1 C27 109.9(2) . . ? C21 Sn1 C33 116.5(2) . . ? C27 Sn1 C33 108.7(3) . . ? C21 Sn1 S1 103.73(16) . . ? C27 Sn1 S1 113.01(18) . . ? C33 Sn1 S1 104.9(2) . . ? C1 Se1 S1 101.30(17) . . ? Se1 S1 Sn1 97.44(6) . . ? C8 C9 C10 119.3(6) . . ? C9 C8 C13 120.5(6) . . ? C9 C8 C1 127.0(5) . . ? C13 C8 C1 112.3(5) . . ? C15 C14 C19 120.2(5) . . ? C15 C14 C1 128.2(5) . . ? C19 C14 C1 111.5(5) . . ? C14 C15 C16 119.3(6) . . ? C6 C5 C4 121.0(7) . . ? C5 C4 C3 118.7(7) . . ? C12 C13 C8 120.3(6) . . ? C12 C13 C20 126.3(6) . . ? C8 C13 C20 113.2(5) . . ? C2 C1 C14 104.9(4) . . ? C2 C1 C8 107.9(4) . . ? C14 C1 C8 105.4(4) . . ? C2 C1 Se1 113.5(4) . . ? C14 C1 Se1 109.0(4) . . ? C8 C1 Se1 115.4(4) . . ? C22 C23 C24 121.3(7) . . ? C30 C31 C32 120.3(7) . . ? C6 C7 C2 119.5(7) . . ? C18 C19 C14 120.7(6) . . ? C18 C19 C20 125.9(6) . . ? C14 C19 C20 113.4(5) . . ? C13 C20 C3 108.3(5) . . ? C13 C20 C19 104.7(5) . . ? C3 C20 C19 105.4(5) . . ? C7 C2 C3 119.4(6) . . ? C7 C2 C1 128.2(6) . . ? C3 C2 C1 112.3(5) . . ? C31 C32 C27 122.4(7) . . ? C13 C12 C11 119.6(6) . . ? C38 C33 C34 116.4(8) . . ? C38 C33 Sn1 123.4(7) . . ? C34 C33 Sn1 120.2(6) . . ? C17 C16 C15 120.9(6) . . ? C25 C26 C21 121.6(7) . . ? C2 C3 C4 120.9(6) . . ? C2 C3 C20 113.3(6) . . ? C4 C3 C20 125.8(6) . . ? C26 C21 C22 117.1(6) . . ? C26 C21 Sn1 120.5(5) . . ? C22 C21 Sn1 122.2(5) . . ? C28 C27 C32 116.8(6) . . ? C28 C27 Sn1 118.7(5) . . ? C32 C27 Sn1 124.5(5) . . ? C19 C18 C17 117.8(6) . . ? C23 C24 C25 118.8(7) . . ? C10 C11 C12 119.2(6) . . ? C9 C10 C11 121.1(7) . . ? C5 C6 C7 120.5(7) . . ? C35 C36 C37 119.5(12) . . ? C31 C30 C29 119.0(8) . . ? C16 C17 C18 121.0(6) . . ? C23 C22 C21 120.8(6) . . ? C26 C25 C24 120.4(7) . . ? C36 C35 C34 120.8(11) . . ? C30 C29 C28 122.1(8) . . ? C27 C28 C29 119.3(7) . . ? C33 C34 C35 122.2(10) . . ? C36 C37 C38 119.8(12) . . ? C33 C38 C37 121.3(11) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 121.6 . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 121.5 . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.6 . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 121.0 . . ? C22 C23 H23 118.2 . . ? C24 C23 H23 120.5 . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 120.1 . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.3 . . ? C13 C20 H20 113.6 . . ? C3 C20 H20 113.8 . . ? C19 C20 H20 110.4 . . ? C31 C32 H32 119.9 . . ? C27 C32 H32 117.7 . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.3 . . ? C17 C16 H16 118.8 . . ? C15 C16 H16 120.3 . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 118.3 . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 123.2 . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 121.7 . . ? C10 C11 H11 121.3 . . ? C12 C11 H11 119.5 . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.6 . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 118.5 . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 120.7 . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.8 . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.4 . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 118.7 . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 119.0 . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 118.2 . . ? C27 C28 H28 118.7 . . ? C29 C28 H28 121.8 . . ? C33 C34 H34 118.1 . . ? C35 C34 H34 119.7 . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 120.7 . . ? C33 C38 H38 118.7 . . ? C37 C38 H38 120.0 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.435 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.081 #===END data_Compound_8 _database_code_CSD 191693 _audit_creation_method 'maXus' _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Cube' _exptl_crystal_colour 'Colorless' _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment 'refxyz' # Submission details _publ_requested_journal 'Chemical Communications' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 682.292 _diffrn_radiation_type ' MoK¥a' loop_ _symmetry_equiv_pos_as_xyz '+X,+Y,+Z' '-X,-Y,-Z' '-X,+Y+ 1/2,-Z+ 1/2' '+X,-Y+ 1/2,+Z+ 1/2' _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_cell_setting 'Monoclinic' _chemical_formula_moiety 'C38 H28 Se Sn ' _chemical_formula_sum 'C38 H28 Se Sn ' _chemical_name_systematic ; Triphenylstannyl 9-triptycyl selenide ; _cell_length_a 9.3690(4) _cell_length_b 24.7190(10) _cell_length_c 13.5380(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.092(3) _cell_angle_gamma 90.00 _cell_volume 3027.2(2) _diffrn_reflns_number 6032 _diffrn_reflns_theta_max 27.13 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_full 27.13 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap # Absorption correction _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.816 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_reflns_av_R_equivalents 0.038 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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _exptl_absorpt_coefficient_mu 2.071 _reflns_number_total 5927 _reflns_number_gt 3957 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0279P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5927 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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 Sn1 Sn 0.80972(3) 0.425922(10) 0.824862(19) 0.04309(10) Uani 1 1 d . . . Se2 Se 0.62910(5) 0.363753(16) 0.70212(3) 0.04589(12) Uani 1 1 d . . . C27 C 0.7627(5) 0.50823(15) 0.7828(3) 0.0449(10) Uani 1 1 d . . . C2 C 0.8595(4) 0.31202(14) 0.6206(3) 0.0412(9) Uani 1 1 d . . . C1 C 0.7186(4) 0.34645(14) 0.5897(2) 0.0365(9) Uani 1 1 d . . . C21 C 1.0365(4) 0.40945(15) 0.8424(3) 0.0476(10) Uani 1 1 d . . . C11 C 0.9264(5) 0.29059(16) 0.7155(3) 0.0501(11) Uani 1 1 d . . . C36 C 0.6722(7) 0.3820(3) 1.1402(4) 0.0819(17) Uani 1 1 d . . . C8 C 0.7633(7) 0.4885(2) 0.4852(4) 0.0830(18) Uani 1 1 d . . . C9 C 0.8298(8) 0.4748(2) 0.4117(4) 0.091(2) Uani 1 1 d . . . C20 C 0.6729(5) 0.29913(15) 0.4273(3) 0.0447(10) Uani 1 1 d . . . C10 C 0.8555(6) 0.4215(2) 0.3930(4) 0.0716(15) Uani 1 1 d . . . C16 C 0.4802(5) 0.29005(16) 0.5120(3) 0.0475(10) Uani 1 1 d . . . C4 C 0.8261(5) 0.32162(18) 0.4387(3) 0.0527(12) Uani 1 1 d . . . C33 C 0.7533(4) 0.40794(15) 0.9632(3) 0.0442(10) Uani 1 1 d . . . C35 C 0.7172(6) 0.3425(2) 1.0856(4) 0.0723(15) Uani 1 1 d . . . C15 C 0.6142(4) 0.31134(13) 0.5087(3) 0.0369(9) Uani 1 1 d . . . C37 C 0.6682(7) 0.4347(3) 1.1085(4) 0.0834(18) Uani 1 1 d . . . C5 C 0.8150(5) 0.38184(16) 0.4514(3) 0.0487(10) Uani 1 1 d . . . C13 C 1.1063(6) 0.2471(2) 0.6468(4) 0.0772(16) Uani 1 1 d . . . C25 C 1.2513(7) 0.4031(2) 0.7796(6) 0.0836(17) Uani 1 1 d . . . C19 C 0.5935(6) 0.26623(18) 0.3485(3) 0.0557(13) Uani 1 1 d . . . C30 C 0.7088(8) 0.6147(2) 0.7209(4) 0.0842(19) Uani 1 1 d . . . C7 C 0.7240(6) 0.44882(18) 0.5458(3) 0.0583(13) Uani 1 1 d . . . C26 C 1.1025(6) 0.41174(17) 0.7619(4) 0.0614(12) Uani 1 1 d . . . C6 C 0.7524(4) 0.39573(15) 0.5308(3) 0.0421(9) Uani 1 1 d . . . C23 C 1.2728(8) 0.3886(3) 0.9542(7) 0.095(2) Uani 1 1 d . . . C3 C 0.9166(5) 0.29934(16) 0.5390(3) 0.0492(10) Uani 1 1 d . . . C17 C 0.4057(6) 0.25599(18) 0.4336(4) 0.0595(13) Uani 1 1 d . . . C28 C 0.8766(6) 0.54514(18) 0.7989(3) 0.0563(12) Uani 1 1 d . . . C24 C 1.3359(8) 0.3912(2) 0.8751(8) 0.096(2) Uani 1 1 d . . . C22 C 1.1244(6) 0.3976(2) 0.9384(4) 0.0690(14) Uani 1 1 d . . . C18 C 0.4621(6) 0.24494(17) 0.3530(4) 0.0601(13) Uani 1 1 d . . . C34 C 0.7571(6) 0.35530(19) 0.9981(3) 0.0592(12) Uani 1 1 d . . . C32 C 0.6209(6) 0.52583(19) 0.7364(4) 0.0617(13) Uani 1 1 d . . . C12 C 1.0497(5) 0.25826(19) 0.7278(4) 0.0658(14) Uani 1 1 d . . . C31 C 0.5943(8) 0.5783(2) 0.7058(4) 0.0816(19) Uani 1 1 d . . . C38 C 0.7082(6) 0.4483(2) 1.0193(3) 0.0620(12) Uani 1 1 d . . . C14 C 1.0399(6) 0.2671(2) 0.5518(4) 0.0682(14) Uani 1 1 d . . . C29 C 0.8498(8) 0.5982(2) 0.7689(4) 0.0801(17) Uani 1 1 d . . . H11 H 0.898(4) 0.2988(14) 0.768(2) 0.036(11) Uiso 1 1 d . . . H36 H 0.644(6) 0.372(2) 1.204(4) 0.11(2) Uiso 1 1 d . . . H8 H 0.745(5) 0.5233(18) 0.497(3) 0.072(15) Uiso 1 1 d . . . H9 H 0.862(5) 0.501(2) 0.371(4) 0.091(16) Uiso 1 1 d . . . H10 H 0.914(5) 0.4110(18) 0.344(4) 0.086(16) Uiso 1 1 d . . . H16 H 0.440(4) 0.2992(13) 0.565(2) 0.037(10) Uiso 1 1 d . . . H4 H 0.860(4) 0.3134(13) 0.391(2) 0.029(10) Uiso 1 1 d . . . H35 H 0.712(5) 0.3062(19) 1.106(3) 0.087(17) Uiso 1 1 d . . . H37 H 0.633(7) 0.464(2) 1.135(4) 0.11(2) Uiso 1 1 d . . . H13 H 1.186(5) 0.2272(18) 0.661(3) 0.069(14) Uiso 1 1 d . . . H25 H 1.287(6) 0.4090(18) 0.721(4) 0.084(18) Uiso 1 1 d . . . H19 H 0.637(5) 0.2600(15) 0.305(3) 0.049(13) Uiso 1 1 d . . . H30 H 0.708(6) 0.653(2) 0.705(4) 0.11(2) Uiso 1 1 d . . . H7 H 0.671(4) 0.4555(14) 0.589(3) 0.040(12) Uiso 1 1 d . . . H26 H 1.045(5) 0.4215(16) 0.693(3) 0.067(13) Uiso 1 1 d . . . H23 H 1.322(7) 0.382(2) 1.017(4) 0.11(2) Uiso 1 1 d . . . H17 H 0.320(5) 0.2414(16) 0.438(3) 0.058(13) Uiso 1 1 d . . . H28 H 0.970(4) 0.5347(13) 0.825(2) 0.030(10) Uiso 1 1 d . . . H24 H 1.427(6) 0.3878(18) 0.880(4) 0.076(18) Uiso 1 1 d . . . H22 H 1.092(5) 0.3978(16) 0.994(3) 0.057(14) Uiso 1 1 d . . . H18 H 0.403(4) 0.2195(16) 0.299(3) 0.061(12) Uiso 1 1 d . . . H34 H 0.796(5) 0.3268(17) 0.962(3) 0.079(15) Uiso 1 1 d . . . H32 H 0.541(5) 0.5032(18) 0.731(3) 0.066(15) Uiso 1 1 d . . . H12 H 1.094(5) 0.2451(16) 0.791(3) 0.068(13) Uiso 1 1 d . . . H31 H 0.512(5) 0.5909(18) 0.675(3) 0.068(15) Uiso 1 1 d . . . H38 H 0.707(5) 0.4858(17) 0.996(3) 0.075(14) Uiso 1 1 d . . . H14 H 1.079(5) 0.2572(17) 0.496(3) 0.081(15) Uiso 1 1 d . . . H29 H 0.934(5) 0.6202(18) 0.784(3) 0.068(15) 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 Sn1 0.04059(19) 0.04164(15) 0.04676(15) 0.00145(13) 0.01083(12) 0.00279(13) Se2 0.0457(3) 0.0500(2) 0.0452(2) -0.00274(18) 0.01758(18) -0.00512(19) C27 0.055(3) 0.037(2) 0.0419(19) -0.0028(17) 0.0099(19) 0.0046(19) C2 0.038(3) 0.038(2) 0.046(2) 0.0032(17) 0.0065(18) 0.0000(17) C1 0.034(2) 0.0393(19) 0.0351(18) -0.0019(16) 0.0070(16) -0.0020(16) C21 0.034(3) 0.039(2) 0.068(3) -0.0013(19) 0.011(2) 0.0000(17) C11 0.056(3) 0.046(2) 0.045(2) -0.001(2) 0.006(2) -0.003(2) C36 0.097(5) 0.099(5) 0.051(3) 0.007(3) 0.020(3) -0.016(3) C8 0.125(5) 0.047(3) 0.069(3) 0.006(3) 0.010(3) -0.022(3) C9 0.125(6) 0.077(4) 0.068(3) 0.023(3) 0.018(3) -0.043(4) C20 0.044(3) 0.044(2) 0.042(2) -0.0015(18) 0.0059(18) 0.0089(18) C10 0.067(4) 0.096(4) 0.055(3) 0.012(3) 0.021(3) -0.022(3) C16 0.038(3) 0.047(2) 0.056(2) -0.001(2) 0.009(2) 0.0029(19) C4 0.053(3) 0.069(3) 0.042(2) -0.002(2) 0.021(2) 0.009(2) C33 0.040(3) 0.051(2) 0.041(2) -0.0015(18) 0.0074(18) -0.0012(18) C35 0.084(4) 0.069(3) 0.061(3) 0.009(3) 0.014(3) -0.008(3) C15 0.032(3) 0.0320(19) 0.044(2) 0.0019(16) 0.0048(17) 0.0039(16) C37 0.098(5) 0.096(5) 0.063(3) -0.021(3) 0.033(3) 0.003(4) C5 0.046(3) 0.058(3) 0.041(2) 0.0091(19) 0.0082(19) -0.007(2) C13 0.049(4) 0.086(4) 0.090(4) -0.001(3) 0.007(3) 0.027(3) C25 0.062(5) 0.071(4) 0.130(6) 0.007(4) 0.046(4) 0.001(3) C19 0.061(4) 0.050(3) 0.053(3) -0.006(2) 0.008(2) 0.013(2) C30 0.126(6) 0.044(3) 0.084(4) 0.009(3) 0.030(4) 0.018(4) C7 0.081(4) 0.045(2) 0.045(2) 0.006(2) 0.009(2) -0.007(2) C26 0.040(3) 0.059(3) 0.088(4) 0.017(3) 0.022(3) 0.001(2) C6 0.040(3) 0.044(2) 0.040(2) 0.0059(17) 0.0051(17) -0.0040(18) C23 0.057(5) 0.093(4) 0.113(6) -0.005(4) -0.016(4) 0.014(3) C3 0.039(3) 0.056(3) 0.051(2) -0.001(2) 0.010(2) 0.002(2) C17 0.037(3) 0.059(3) 0.077(3) -0.007(2) 0.006(3) -0.009(2) C28 0.049(3) 0.053(3) 0.067(3) 0.000(2) 0.014(2) 0.003(2) C24 0.038(5) 0.073(4) 0.174(8) -0.001(4) 0.019(5) 0.006(3) C22 0.051(4) 0.074(3) 0.072(3) -0.005(3) -0.003(3) 0.011(3) C18 0.052(3) 0.048(3) 0.070(3) -0.014(2) -0.003(3) 0.003(2) C34 0.069(4) 0.059(3) 0.048(2) -0.002(2) 0.014(2) -0.003(2) C32 0.055(4) 0.054(3) 0.073(3) -0.005(2) 0.010(3) 0.012(3) C12 0.054(4) 0.064(3) 0.066(3) 0.010(3) -0.008(3) 0.012(2) C31 0.093(5) 0.072(4) 0.070(3) 0.002(3) 0.004(3) 0.046(4) C38 0.067(4) 0.062(3) 0.060(3) -0.004(2) 0.021(2) 0.001(3) C14 0.045(3) 0.090(4) 0.067(3) -0.010(3) 0.011(3) 0.013(3) C29 0.097(5) 0.049(3) 0.097(4) -0.001(3) 0.029(4) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C21 2.115(4) . ? Sn1 C33 2.122(4) . ? Sn1 C27 2.128(4) . ? Sn1 Se2 2.5538(5) . ? Se2 C1 1.966(3) . ? C27 C28 1.377(6) . ? C27 C32 1.383(6) . ? C2 C11 1.380(5) . ? C2 C3 1.383(5) . ? C2 C1 1.534(5) . ? C1 C6 1.534(5) . ? C1 C15 1.535(5) . ? C21 C22 1.378(6) . ? C21 C26 1.387(6) . ? C11 C12 1.379(6) . ? C36 C35 1.355(7) . ? C36 C37 1.371(8) . ? C8 C9 1.348(8) . ? C8 C7 1.388(7) . ? C9 C10 1.376(8) . ? C20 C15 1.388(5) . ? C20 C19 1.393(6) . ? C20 C4 1.509(6) . ? C10 C5 1.373(6) . ? C16 C15 1.373(5) . ? C16 C17 1.391(6) . ? C4 C5 1.505(6) . ? C4 C3 1.506(5) . ? C33 C34 1.381(5) . ? C33 C38 1.385(6) . ? C35 C34 1.369(6) . ? C37 C38 1.395(7) . ? C5 C6 1.395(5) . ? C13 C12 1.364(7) . ? C13 C14 1.368(7) . ? C25 C24 1.361(10) . ? C25 C26 1.368(7) . ? C19 C18 1.354(7) . ? C30 C29 1.373(8) . ? C30 C31 1.374(8) . ? C7 C6 1.365(6) . ? C23 C24 1.353(10) . ? C23 C22 1.369(8) . ? C3 C14 1.377(6) . ? C17 C18 1.358(6) . ? C28 C29 1.377(7) . ? C32 C31 1.364(7) . ? C11 H11 0.84(3) . ? C36 H36 1.00(5) . ? C8 H8 0.90(4) . ? C9 H9 0.95(5) . ? C10 H10 1.00(5) . ? C16 H16 0.92(3) . ? C4 H4 0.81(3) . ? C35 H35 0.94(5) . ? C37 H37 0.90(5) . ? C13 H13 0.87(4) . ? C25 H25 0.95(5) . ? C19 H19 0.81(4) . ? C30 H30 0.97(6) . ? C7 H7 0.88(4) . ? C26 H26 0.98(4) . ? C23 H23 0.87(5) . ? C17 H17 0.89(4) . ? C28 H28 0.89(3) . ? C24 H24 0.85(5) . ? C22 H22 0.88(4) . ? C18 H18 1.01(4) . ? C34 H34 0.98(4) . ? C32 H32 0.92(4) . ? C12 H12 0.91(4) . ? C31 H31 0.84(4) . ? C38 H38 0.98(4) . ? C14 H14 0.96(4) . ? C29 H29 0.94(4) . ? 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 Sn1 C33 109.56(16) . . ? C21 Sn1 C27 110.23(16) . . ? C33 Sn1 C27 110.79(15) . . ? C21 Sn1 Se2 115.67(10) . . ? C33 Sn1 Se2 99.97(10) . . ? C27 Sn1 Se2 110.20(11) . . ? C1 Se2 Sn1 106.89(10) . . ? C28 C27 C32 118.5(4) . . ? C28 C27 Sn1 119.5(3) . . ? C32 C27 Sn1 122.0(3) . . ? C11 C2 C3 118.7(4) . . ? C11 C2 C1 128.0(4) . . ? C3 C2 C1 113.1(3) . . ? C6 C1 C2 107.6(3) . . ? C6 C1 C15 104.9(3) . . ? C2 C1 C15 102.9(3) . . ? C6 C1 Se2 114.7(2) . . ? C2 C1 Se2 114.8(2) . . ? C15 C1 Se2 110.8(2) . . ? C22 C21 C26 118.1(5) . . ? C22 C21 Sn1 118.9(4) . . ? C26 C21 Sn1 123.0(3) . . ? C12 C11 C2 119.9(5) . . ? C35 C36 C37 120.0(5) . . ? C9 C8 C7 120.3(6) . . ? C8 C9 C10 120.8(5) . . ? C15 C20 C19 119.5(4) . . ? C15 C20 C4 113.7(3) . . ? C19 C20 C4 126.7(4) . . ? C5 C10 C9 119.4(5) . . ? C15 C16 C17 119.2(4) . . ? C5 C4 C3 107.3(3) . . ? C5 C4 C20 106.5(4) . . ? C3 C4 C20 104.8(3) . . ? C34 C33 C38 118.5(4) . . ? C34 C33 Sn1 120.6(3) . . ? C38 C33 Sn1 121.0(3) . . ? C36 C35 C34 120.0(5) . . ? C16 C15 C20 119.8(4) . . ? C16 C15 C1 127.7(3) . . ? C20 C15 C1 112.3(3) . . ? C36 C37 C38 120.6(5) . . ? C10 C5 C6 120.2(4) . . ? C10 C5 C4 127.0(4) . . ? C6 C5 C4 112.8(3) . . ? C12 C13 C14 120.4(5) . . ? C24 C25 C26 121.0(7) . . ? C18 C19 C20 120.2(5) . . ? C29 C30 C31 119.6(5) . . ? C6 C7 C8 120.0(5) . . ? C25 C26 C21 119.9(6) . . ? C7 C6 C5 119.3(4) . . ? C7 C6 C1 127.7(4) . . ? C5 C6 C1 113.0(3) . . ? C24 C23 C22 120.3(7) . . ? C14 C3 C2 121.2(4) . . ? C14 C3 C4 125.6(4) . . ? C2 C3 C4 113.2(4) . . ? C18 C17 C16 120.8(5) . . ? C29 C28 C27 120.6(5) . . ? C23 C24 C25 119.7(7) . . ? C23 C22 C21 121.0(6) . . ? C19 C18 C17 120.4(5) . . ? C35 C34 C33 121.6(5) . . ? C31 C32 C27 121.0(5) . . ? C13 C12 C11 120.6(5) . . ? C32 C31 C30 120.2(6) . . ? C33 C38 C37 119.3(5) . . ? C13 C14 C3 119.3(5) . . ? C30 C29 C28 120.1(6) . . ? C12 C11 H11 119(2) . . ? C2 C11 H11 121(2) . . ? C35 C36 H36 118(3) . . ? C37 C36 H36 122(3) . . ? C9 C8 H8 121(3) . . ? C7 C8 H8 119(3) . . ? C8 C9 H9 122(3) . . ? C10 C9 H9 117(3) . . ? C5 C10 H10 119(3) . . ? C9 C10 H10 122(3) . . ? C15 C16 H16 119(2) . . ? C17 C16 H16 121(2) . . ? C5 C4 H4 113(2) . . ? C3 C4 H4 112(2) . . ? C20 C4 H4 113(3) . . ? C36 C35 H35 118(3) . . ? C34 C35 H35 122(3) . . ? C36 C37 H37 128(4) . . ? C38 C37 H37 111(4) . . ? C12 C13 H13 115(3) . . ? C14 C13 H13 124(3) . . ? C24 C25 H25 126(3) . . ? C26 C25 H25 113(3) . . ? C18 C19 H19 126(3) . . ? C20 C19 H19 113(3) . . ? C29 C30 H30 110(3) . . ? C31 C30 H30 130(3) . . ? C6 C7 H7 117(2) . . ? C8 C7 H7 123(2) . . ? C25 C26 H26 119(3) . . ? C21 C26 H26 121(3) . . ? C24 C23 H23 124(4) . . ? C22 C23 H23 116(4) . . ? C18 C17 H17 121(3) . . ? C16 C17 H17 118(3) . . ? C29 C28 H28 119(2) . . ? C27 C28 H28 121(2) . . ? C23 C24 H24 125(4) . . ? C25 C24 H24 115(4) . . ? C23 C22 H22 116(3) . . ? C21 C22 H22 123(3) . . ? C19 C18 H18 123(2) . . ? C17 C18 H18 116(2) . . ? C35 C34 H34 119(3) . . ? C33 C34 H34 119(3) . . ? C31 C32 H32 118(3) . . ? C27 C32 H32 120(3) . . ? C13 C12 H12 120(3) . . ? C11 C12 H12 119(3) . . ? C32 C31 H31 125(3) . . ? C30 C31 H31 114(3) . . ? C33 C38 H38 119(3) . . ? C37 C38 H38 122(3) . . ? C13 C14 H14 119(3) . . ? C3 C14 H14 122(3) . . ? C30 C29 H29 126(3) . . ? C28 C29 H29 114(3) . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_measured_fraction_theta_full 0.886 _refine_diff_density_max 0.287 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.078 #===END