Supplementary Material (ESI) for CrystEngComm This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name _publ_author_address 'Claborn, Kacey' ; Department of Chemistry University of Washington Seattle, WA 98195 USA ; 'Kahr, Bart' ; Department of Chemistry University of Washington Seattle, WA 98195 USA ; 'Kaminsky, Werner' ; Department of Chemistry University of Washington Seattle, WA 98195 USA ; _publ_contact_author_name 'Dr Werner Kaminsky' _publ_contact_author_address ; Department of Chemistry University of Washington Seattle WA 98195-1700 UNITED STATES OF AMERICA ; _publ_contact_email 'Kaminsky@WinTensor.com' _publ_requested_journal 'Cryst. Eng. Comm.' _publ_section_title ; Calculations of optical properties of the tetraphenyl-X family of isomorphous crystals (X=3DX, Si, Ge, Sn, Pb) ; data_Ph4Pb _database_code_CSD 185087 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Ph4Pb' ; _chemical_name_common 'Ph4Pb' _chemical_formula_moiety 'C6 H5 Pb0.25' _chemical_formula_sum 'C6 H5 Pb0.25' _chemical_formula_weight 128.90 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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 12.1110(9) _cell_length_b 12.1110(9) _cell_length_c 6.5430(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 959.70(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 369 _exptl_crystal_description 'parallelepiped' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 8.792 _exptl_absorpt_correction_type 'numerical, HKL-scalepack' _exptl_absorpt_correction_T_min 0.0730 _exptl_absorpt_correction_T_max 0.2172 _exptl_special_details ; Data was collected with \w and \f scans in 2^o^ increments with 20 second exposures per degree. Crystal-to-detector distance was 25 mm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 654 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 23.25 _reflns_number_total 654 _reflns_number_gt 524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL SCALEPACK' _computing_data_reduction 'DENZO' _computing_structure_solution 'SIR92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus, Zortep' _computing_publication_material '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. Those H atoms that where placed were refined with a riding model. U~iso~ values were fixed such that they were 1.2U~eq7~ of their parent atom U~eq~ for CH's and 1.5U~eq~ of their parent atom U~eq~ in case of methyl groups. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme ; calc w=3D1/[\s^2^(Fo^2^)+(0.1121P)^2^+0.0000P] where P=3D(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'H atoms riding' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.065(10) _refine_ls_extinction_expression 'Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(14) _refine_ls_number_reflns 654 _refine_ls_number_parameters 59 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.0220(7) 0.1502(8) 0.1922(13) 0.051(2) Uani 1 d . . . C3 C -0.0537(7) 0.2353(8) 0.1726(14) 0.057(3) Uani 1 d . . . H2 H -0.1114 0.2300 0.0795 0.068 Uiso 1 calc R . . C4 C -0.0423(9) 0.3278(8) 0.2929(14) 0.069(3) Uani 1 d . . . H4 H -0.0919 0.3860 0.2795 0.082 Uiso 1 calc R . . C5 C 0.0425(11) 0.3346(10) 0.4335(16) 0.070(3) Uani 1 d . . . H5 H 0.0499 0.3970 0.5152 0.083 Uiso 1 calc R . . C6 C 0.1145(9) 0.2504(9) 0.4517(17) 0.068(3) Uani 1 d . . . H6 H 0.1725 0.2560 0.5445 0.082 Uiso 1 calc R . . C7 C 0.1034(11) 0.1529(12) 0.331(2) 0.060(3) Uani 1 d . . . H7 H 0.1509 0.0933 0.3481 0.072 Uiso 1 calc R . . Pb1 Pb 0.0000 0.0000 0.0000 0.0461(8) Uani 1 d S . . 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 C2 0.050(5) 0.055(6) 0.049(4) 0.004(5) 0.000(5) -0.001(4) C3 0.055(6) 0.061(6) 0.055(5) -0.001(5) -0.005(5) 0.011(5) C4 0.080(7) 0.059(7) 0.066(5) 0.001(6) 0.010(7) 0.028(6) C5 0.089(8) 0.058(7) 0.061(5) -0.005(5) 0.012(7) -0.015(7) C6 0.068(7) 0.074(7) 0.063(6) -0.005(7) -0.011(6) -0.023(6) C7 0.055(7) 0.060(8) 0.065(7) 0.004(7) -0.005(7) 0.003(5) Pb1 0.0457(8) 0.0457(8) 0.0469(9) 0.000 0.000 0.000 _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 C2 C7 1.341(16) . ? C2 C3 1.386(12) . ? C2 Pb1 2.227(9) . ? C3 C4 1.376(14) . ? C3 H2 0.9300 . ? C4 C5 1.382(15) . ? C4 H4 0.9300 . ? C5 C6 1.346(18) . ? C5 H5 0.9300 . ? C6 C7 1.427(18) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? Pb1 C2 2.227(9) 7 ? Pb1 C2 2.227(9) 2 ? Pb1 C2 2.227(9) 8 ? 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 C7 C2 C3 122.0(11) . . ? C7 C2 Pb1 119.4(8) . . ? C3 C2 Pb1 118.5(7) . . ? C4 C3 C2 119.1(9) . . ? C4 C3 H2 120.4 . . ? C2 C3 H2 120.4 . . ? C3 C4 C5 120.2(8) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 119.8(10) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 121.0(11) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 117.7(12) . . ? C2 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C2 Pb1 C2 108.6(2) 7 . ? C2 Pb1 C2 108.6(2) 7 2 ? C2 Pb1 C2 111.3(5) . 2 ? C2 Pb1 C2 111.3(5) 7 8 ? C2 Pb1 C2 108.6(2) . 8 ? C2 Pb1 C2 108.6(2) 2 8 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 2.170 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.175 data_Ph4Sn _database_code_CSD 185088 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Ph4Sn' ; _chemical_name_common 'Ph4Sn' _chemical_formula_moiety 'C6 H5 Sn0.25' _chemical_formula_sum 'C6 H5 Sn0.25' _chemical_formula_weight 427.09 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' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 12.0680(4) _cell_length_b 12.0680(4) _cell_length_c 6.5570(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 954.94(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 422 _exptl_crystal_description 'parallelepiped' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type 'Sortav' _exptl_absorpt_correction_T_min 0.7661 _exptl_absorpt_correction_T_max 0.7848 _exptl_special_details ; Data was collected with \w and \f scans in 2^o^ increments with 10 second exposures per degree. Crystal-to-detector distance was 27 mm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 960 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 26.37 _reflns_number_total 960 _reflns_number_gt 784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'DENZO' _computing_structure_solution 'SIR92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus, Zortep' _computing_publication_material '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 w=3D1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.0630P] where P=3D(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'full-isotropic' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.083(6) _refine_ls_extinction_expression 'Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.09(8) _refine_ls_number_reflns 960 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0671 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C -0.0189(2) 0.1451(3) 0.1852(4) 0.0478(8) Uani 1 d . . . C3 C 0.0539(3) 0.2333(3) 0.1674(5) 0.0552(8) Uani 1 d . . . H3 H 0.118(3) 0.233(3) 0.070(7) 0.063(10) Uiso 1 d . . . C4 C 0.0424(4) 0.3265(3) 0.2876(6) 0.0660(9) Uani 1 d . . . H4 H 0.094(4) 0.379(4) 0.272(7) 0.091(14) Uiso 1 d . . . C5 C -0.0419(4) 0.3342(3) 0.4257(6) 0.0669(10) Uani 1 d . . . H5 H -0.048(4) 0.399(4) 0.505(6) 0.081(11) Uiso 1 d . . . C6 C -0.1159(4) 0.2479(3) 0.4454(6) 0.0662(10) Uani 1 d . . . H6 H -0.173(3) 0.252(3) 0.542(7) 0.072(12) Uiso 1 d . . . C7 C -0.1043(4) 0.1540(4) 0.3264(7) 0.0565(9) Uani 1 d . . . H7 H -0.159(3) 0.095(3) 0.338(5) 0.040(8) Uiso 1 d . . . Sn1 Sn 0.0000 0.0000 0.0000 0.0445(2) Uani 1 d S . . 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 C2 0.0486(19) 0.0468(16) 0.0481(15) -0.0005(13) 0.0000(14) 0.0003(13) C3 0.0572(19) 0.055(2) 0.0537(19) -0.0020(16) 0.0022(18) -0.0068(17) C4 0.078(2) 0.052(2) 0.068(2) 0.0027(19) -0.006(2) -0.0128(18) C5 0.083(3) 0.055(2) 0.063(2) -0.0106(17) -0.009(2) 0.014(2) C6 0.064(2) 0.076(3) 0.058(2) -0.0039(18) 0.0090(17) 0.015(2) C7 0.053(2) 0.059(2) 0.058(2) 0.0025(19) 0.0022(18) -0.0024(17) Sn1 0.0424(2) 0.0424(2) 0.0487(3) 0.000 0.000 0.000 _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 C2 C3 1.385(4) . ? C2 C7 1.390(5) . ? C2 Sn1 2.143(3) . ? C3 C4 1.380(5) . ? C3 H3 1.01(4) . ? C4 C5 1.365(6) . ? C4 H4 0.89(5) . ? C5 C6 1.378(6) . ? C5 H5 0.94(4) . ? C6 C7 1.384(6) . ? C6 H6 0.94(4) . ? C7 H7 0.98(4) . ? Sn1 C2 2.143(3) 7 ? Sn1 C2 2.143(3) 8 ? Sn1 C2 2.143(3) 2 ? 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 C3 C2 C7 117.8(3) . . ? C3 C2 Sn1 120.9(2) . . ? C7 C2 Sn1 121.3(3) . . ? C4 C3 C2 121.0(3) . . ? C4 C3 H3 117(2) . . ? C2 C3 H3 122(2) . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 123(3) . . ? C3 C4 H4 116(3) . . ? C4 C5 C6 119.6(4) . . ? C4 C5 H5 119(3) . . ? C6 C5 H5 122(3) . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H6 120(3) . . ? C7 C6 H6 120(3) . . ? C6 C7 C2 120.9(4) . . ? C6 C7 H7 119(2) . . ? C2 C7 H7 120(2) . . ? C2 Sn1 C2 110.94(17) 7 8 ? C2 Sn1 C2 108.74(8) 7 . ? C2 Sn1 C2 108.74(8) 8 . ? C2 Sn1 C2 108.74(8) 7 2 ? C2 Sn1 C2 108.74(8) 8 2 ? C2 Sn1 C2 110.94(17) . 2 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.298 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.047 data_Ph4Ge _database_code_CSD 185089 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Ph4Ge' ; _chemical_name_common 'Ph4Ge' _chemical_formula_moiety 'C6 H5 Ge0.25' _chemical_formula_sum 'C6 H5 Ge0.25' _chemical_formula_weight 380.99 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' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 11.6160(5) _cell_length_b 11.616 _cell_length_c 6.9020(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 931.30(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 318 _exptl_crystal_description 'prism' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 1.647 _exptl_absorpt_correction_type 'HKL-Scalepack' _exptl_absorpt_correction_T_min 0.5053 _exptl_absorpt_correction_T_max 0.9401 _exptl_special_details ; Data was collected with \w and \f scans in 2^o^ increments with 15 second exposures per degree. Crystal-to-detector distance was 30 mm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 912 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 26.37 _reflns_number_total 912 _reflns_number_gt 767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'DENZO' _computing_structure_solution 'SIR92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus, Zortep' _computing_publication_material '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 w=3D1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.1306P] where P=3D(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'full-isotropic' _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 0.00(12) _refine_ls_number_reflns 912 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C -0.0167(3) 0.1353(3) 0.1653(5) 0.0447(8) Uani 1 d . . . C3 C 0.0542(3) 0.2313(3) 0.1464(6) 0.0529(8) Uani 1 d . . . H3 H 0.119(4) 0.237(4) 0.050(6) 0.064 Uiso 1 d . . . C4 C 0.0403(5) 0.3259(4) 0.2633(6) 0.0646(11) Uani 1 d . . . H4 H 0.090(4) 0.392(5) 0.244(6) 0.078 Uiso 1 d . . . C5 C -0.0447(4) 0.3284(4) 0.3996(6) 0.0643(11) Uani 1 d . . . H5 H -0.058(4) 0.388(5) 0.476(7) 0.077 Uiso 1 d . . . C6 C -0.1149(4) 0.2352(5) 0.4216(6) 0.0647(12) Uani 1 d . . . H6 H -0.165(5) 0.232(5) 0.507(9) 0.078 Uiso 1 d . . . C7 C -0.1015(4) 0.1385(4) 0.3075(7) 0.0577(11) Uani 1 d . . . H7 H -0.144(5) 0.068(5) 0.350(8) 0.069 Uiso 1 d . . . Ge1 Ge 0.0000 0.0000 0.0000 0.0432(3) Uani 1 d S . . 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 C2 0.0398(18) 0.0410(16) 0.0532(16) 0.0036(14) -0.0038(15) 0.0007(13) C3 0.0504(18) 0.0492(18) 0.0592(19) -0.0006(16) 0.0030(17) -0.0062(17) C4 0.079(3) 0.042(2) 0.073(3) -0.0029(18) -0.007(2) -0.0073(19) C5 0.083(3) 0.052(2) 0.057(2) -0.0102(19) -0.006(2) 0.014(2) C6 0.061(3) 0.080(3) 0.053(2) -0.002(2) 0.0059(18) 0.015(3) C7 0.052(2) 0.059(3) 0.063(3) 0.005(2) 0.001(2) -0.0024(19) Ge1 0.0244(5) 0.050 0.0551(5) 0.000 0.000 0.000 _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 C2 C7 1.391(6) . ? C2 C3 1.393(5) . ? C2 Ge1 1.952(3) . ? C3 C4 1.373(6) . ? C3 H3 1.00(4) . ? C4 C5 1.364(7) . ? C4 H4 0.96(6) . ? C5 C6 1.363(7) . ? C5 H5 0.88(5) . ? C6 C7 1.381(7) . ? C6 H6 0.83(6) . ? C7 H7 1.00(5) . ? Ge1 C2 1.952(3) 7 ? Ge1 C2 1.952(3) 2 ? Ge1 C2 1.952(3) 8 ? 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 C7 C2 C3 117.6(3) . . ? C7 C2 Ge1 120.3(3) . . ? C3 C2 Ge1 122.1(3) . . ? C4 C3 C2 121.1(4) . . ? C4 C3 H3 115(3) . . ? C2 C3 H3 124(3) . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4 121(3) . . ? C3 C4 H4 119(3) . . ? C6 C5 C4 119.5(4) . . ? C6 C5 H5 117(3) . . ? C4 C5 H5 124(3) . . ? C5 C6 C7 121.0(4) . . ? C5 C6 H6 123(4) . . ? C7 C6 H6 116(4) . . ? C6 C7 C2 120.2(4) . . ? C6 C7 H7 117(3) . . ? C2 C7 H7 122(3) . . ? C2 Ge1 C2 109.99(10) 7 2 ? C2 Ge1 C2 108.4(2) 7 8 ? C2 Ge1 C2 109.99(10) 2 8 ? C2 Ge1 C2 109.99(10) 7 . ? C2 Ge1 C2 108.4(2) 2 . ? C2 Ge1 C2 109.99(10) 8 . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.446 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.166 data_Ph4Si _database_code_CSD 185090 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Ph4Si' ; _chemical_name_common 'Ph4Si' _chemical_formula_moiety 'C6 H5 Si0.25' _chemical_formula_sum 'C6 H5 Si0.25' _chemical_formula_weight 84.12 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_cell_setting 'Tetragonal' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 11.4476(9) _cell_length_b 11.4476(9) _cell_length_c 7.0644(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 925.77(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 421 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type 'HKL-Scalepack' _exptl_absorpt_correction_T_min 0.9453 _exptl_absorpt_correction_T_max 0.9784 _exptl_special_details ; Data was collected with an \f scan in 2^o^ increments with 10 second exposures per degree. Crystal-to-detector distance was 30 mm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scan' _diffrn_reflns_number 771 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 24.69 _reflns_number_total 771 _reflns_number_gt 660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL SCALEPACK' _computing_data_reduction 'DENZO' _computing_structure_solution 'SIR92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus, Zortep' _computing_publication_material '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. Hydrogens are located from the Fourier and rifined full, with isotropic thermal parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme ; calc w=3D1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0724P] where P=3D(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'full-isotropic' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.05(2) _refine_ls_extinction_expression 'Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(3) _refine_ls_number_reflns 771 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C -0.01589(19) 0.13142(17) 0.1558(3) 0.0508(6) Uani 1 d . . . C3 C 0.0529(2) 0.2307(2) 0.1369(3) 0.0626(6) Uani 1 d . . . H3 H 0.114(2) 0.236(2) 0.044(4) 0.079(8) Uiso 1 d . . . C4 C 0.0384(3) 0.3260(2) 0.2539(4) 0.0722(8) Uani 1 d . . . H4 H 0.088(2) 0.393(3) 0.231(4) 0.087(8) Uiso 1 d . . . C5 C -0.0455(3) 0.3261(3) 0.3903(4) 0.0736(8) Uani 1 d . . . H5 H -0.0553(19) 0.390(2) 0.479(4) 0.086(8) Uiso 1 d . . . C6 C -0.1144(3) 0.2297(3) 0.4141(4) 0.0730(8) Uani 1 d . . . H6 H -0.173(2) 0.221(2) 0.517(4) 0.075(7) Uiso 1 d . . . C7 C -0.0997(2) 0.1333(3) 0.2980(3) 0.0640(7) Uani 1 d . . . H7 H -0.144(2) 0.070(2) 0.320(3) 0.068(7) Uiso 1 d . . . Si1 Si 0.0000 0.0000 0.0000 0.0518(4) Uani 1 d S . . 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 C2 0.0468(13) 0.0495(12) 0.0562(10) 0.0042(9) -0.0042(10) 0.0021(10) C3 0.0627(15) 0.0604(15) 0.0646(13) -0.0024(12) 0.0024(12) -0.0055(12) C4 0.087(2) 0.0529(15) 0.0768(15) -0.0046(13) -0.0085(15) -0.0078(13) C5 0.0888(19) 0.0668(18) 0.0651(15) -0.0134(13) -0.0088(14) 0.0160(16) C6 0.0683(18) 0.090(2) 0.0608(14) -0.0040(14) 0.0057(13) 0.0129(16) C7 0.0612(15) 0.0647(17) 0.0663(14) 0.0038(13) 0.0059(13) -0.0025(13) Si1 0.0453(9) 0.050 0.0599(6) 0.000 0.000 0.000 _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 C2 C3 1.389(3) . ? C2 C7 1.389(3) . ? C2 Si1 1.8730(19) . ? C3 C4 1.379(3) . ? C3 H3 0.96(3) . ? C4 C5 1.361(4) . ? C4 H4 0.97(3) . ? C5 C6 1.366(4) . ? C5 H5 0.97(3) . ? C6 C7 1.385(4) . ? C6 H6 0.99(3) . ? C7 H7 0.90(2) . ? Si1 C2 1.8730(19) 7 ? Si1 C2 1.8730(19) 2 ? Si1 C2 1.8730(19) 8 ? 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 C3 C2 C7 116.6(2) . . ? C3 C2 Si1 123.05(16) . . ? C7 C2 Si1 120.31(18) . . ? C4 C3 C2 121.4(2) . . ? C4 C3 H3 116.4(16) . . ? C2 C3 H3 122.2(16) . . ? C5 C4 C3 120.7(3) . . ? C5 C4 H4 121.8(15) . . ? C3 C4 H4 117.4(16) . . ? C4 C5 C6 119.6(2) . . ? C4 C5 H5 122.7(14) . . ? C6 C5 H5 117.5(14) . . ? C5 C6 C7 120.0(3) . . ? C5 C6 H6 124.0(14) . . ? C7 C6 H6 115.8(15) . . ? C6 C7 C2 121.6(3) . . ? C6 C7 H7 118.2(15) . . ? C2 C7 H7 120.1(15) . . ? C2 Si1 C2 110.20(6) 7 . ? C2 Si1 C2 110.20(6) 7 2 ? C2 Si1 C2 108.02(12) . 2 ? C2 Si1 C2 108.02(12) 7 8 ? C2 Si1 C2 110.20(6) . 8 ? C2 Si1 C2 110.20(6) 2 8 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.109 _refine_diff_density_min -0.131 _refine_diff_density_rms 0.026 data_Ph4C _database_code_CSD 185091 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Ph4C' ; _chemical_name_common 'Ph4C' _chemical_formula_moiety 'C6.25 H5' _chemical_formula_sum 'C6.25 H5' _chemical_formula_weight 80.10 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 10.9050(10) _cell_length_b 10.9050(10) _cell_length_c 7.2850(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 866.33(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 166 _exptl_crystal_description 'cut needle' _exptl_crystal_colour 'brownish-clear' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type 'HKL-Scalepack' _exptl_absorpt_correction_T_min 0.9883 _exptl_absorpt_correction_T_max 0.9924 _exptl_special_details ; Data was collected with a \f scan in 2^o^ increments with 20 second exposures per degree. Crystal-to-detector distance was 30 mm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 733 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 24.68 _reflns_number_total 733 _reflns_number_gt 555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL SCALEPACK' _computing_data_reduction 'DENZO' _computing_structure_solution 'SIR92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus, Zortep' _computing_publication_material '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. Hydrogens are located from the Fourier map and are rifined full, with isotropic thermal parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme ; calc w=3D1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0880P] where P=3D(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'full-isotropic' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.082(15) _refine_ls_extinction_expression 'Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_ls_number_reflns 733 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0000 0.0000 0.0000 0.0416(10) Uani 1 d S . . C2 C -0.01423(19) 0.11311(19) 0.1269(3) 0.0431(6) Uani 1 d . . . C3 C 0.0523(2) 0.2202(2) 0.1087(3) 0.0516(7) Uani 1 d . . . H3 H 0.114(2) 0.225(2) 0.012(4) 0.073(8) Uiso 1 d . . . C4 C 0.0355(3) 0.3180(2) 0.2268(3) 0.0617(8) Uani 1 d . . . H4 H 0.078(2) 0.387(2) 0.208(3) 0.061(8) Uiso 1 d . . . C5 C -0.0496(3) 0.3116(3) 0.3648(4) 0.0654(8) Uani 1 d . . . H5 H -0.0643(19) 0.377(2) 0.441(3) 0.068(8) Uiso 1 d . . . C6 C -0.1158(3) 0.2053(3) 0.3887(4) 0.0614(8) Uani 1 d . . . H6 H -0.169(2) 0.198(2) 0.486(5) 0.059(7) Uiso 1 d . . . C7 C -0.0981(2) 0.1078(3) 0.2719(3) 0.0529(7) Uani 1 d . . . H7 H -0.141(2) 0.042(2) 0.289(3) 0.039(6) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(3) 0.047 0.0398(19) 0.000 0.000 0.000 C2 0.0431(12) 0.0456(13) 0.0405(9) -0.0012(11) -0.0050(11) 0.0030(10) C3 0.0552(15) 0.0500(14) 0.0497(14) -0.0035(13) 0.0011(14) -0.0003(11) C4 0.0758(19) 0.0472(17) 0.0622(16) -0.0057(14) -0.0089(15) -0.0045(14) C5 0.078(2) 0.0596(18) 0.0592(15) -0.0171(15) -0.0097(16) 0.0137(17) C6 0.0584(17) 0.078(2) 0.0480(14) -0.0058(15) 0.0001(15) 0.0151(15) C7 0.0528(15) 0.0546(16) 0.0515(14) -0.0029(13) 0.0027(12) -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 C1 C2 1.549(2) . ? C1 C2 1.549(2) 2 ? C1 C2 1.549(2) 8 ? C1 C2 1.549(2) 7 ? C2 C3 1.382(3) . ? C2 C7 1.399(3) . ? C3 C4 1.382(3) . ? C3 H3 0.97(3) . ? C4 C5 1.370(4) . ? C4 H4 0.89(3) . ? C5 C6 1.377(4) . ? C5 H5 0.92(3) . ? C6 C7 1.375(4) . ? C6 H6 0.92(3) . ? C7 H7 0.86(2) . ? 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 C2 C1 C2 106.74(15) . 2 ? C2 C1 C2 110.85(8) . 8 ? C2 C1 C2 110.85(8) 2 8 ? C2 C1 C2 110.85(8) . 7 ? C2 C1 C2 110.85(8) 2 7 ? C2 C1 C2 106.74(15) 8 7 ? C3 C2 C7 116.8(2) . . ? C3 C2 C1 124.29(19) . . ? C7 C2 C1 118.90(17) . . ? C2 C3 C4 121.5(3) . . ? C2 C3 H3 118.4(16) . . ? C4 C3 H3 120.0(16) . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 120.7(15) . . ? C3 C4 H4 118.8(15) . . ? C4 C5 C6 119.4(3) . . ? C4 C5 H5 121.4(15) . . ? C6 C5 H5 119.2(14) . . ? C7 C6 C5 120.0(3) . . ? C7 C6 H6 119.9(16) . . ? C5 C6 H6 120.0(16) . . ? C6 C7 C2 121.8(3) . . ? C6 C7 H7 118.3(14) . . ? C2 C7 H7 119.9(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.132 _refine_diff_density_min -0.171 _refine_diff_density_rms 0.053