data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Palmer, Benjamin' 'Kariuki, Benson' 'Muppidi, Vamsee' 'Hughes, Colan' 'Harris, Kenneth' _publ_contact_author_name 'Kenneth Harris' _publ_contact_author_address ; Park Place Cardiff CF10 3AT ; _publ_contact_author_email HarrisKDM@cardiff.ac.uk data_kdm1029 _database_code_depnum_ccdc_archive 'CCDC 804311' #TrackingRef '- BIB_thiourea.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C H4 N2 S, C3.18' _chemical_formula_sum 'C4.18 H4 N2 S' _chemical_formula_weight 114.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 15.6697(6) _cell_length_b 15.6697(6) _cell_length_c 12.4688(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2651.41(17) _cell_formula_units_Z 18 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 518 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.42 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8493 _exptl_absorpt_correction_T_max 0.9018 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3600 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.42 _reflns_number_total 668 _reflns_number_gt 518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997' _computing_structure_solution 'Sir-92 (A. Altomare et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-99 for Windows (Farrugia, 1995)' _computing_publication_material 'WinGX publication routines (Farrugia, 1995)' _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^)+(0.0609P)^2^+2.6546P] 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 SHELXL _refine_ls_extinction_coef 0.011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 668 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _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 S1 S 0.29584(5) 0.0000 0.2500 0.0596(5) Uani 1 2 d S . . N1 N 0.44044(18) -0.01449(19) 0.16017(13) 0.0780(8) Uani 1 1 d . . . H1A H 0.4967 -0.0144 0.1609 0.094 Uiso 1 1 calc R . . H1B H 0.4080 -0.0243 0.0996 0.094 Uiso 1 1 calc R . . C1 C 0.4048(2) 0.0000 0.2500 0.0573(8) Uani 1 2 d S . . C2 C 0.5656 0.2974 0.2769 0.167(17) Uiso 0.12 1 d P . . C3 C 0.6279 0.3051 0.2178 0.171(3) Uiso 0.83 1 d P . . C4 C 0.6667 0.3333 0.2979 0.092(6) Uiso 0.27 3 d SP . . C5 C 0.6667 0.3333 0.0833 0.114(3) Uiso 0.29 6 d SP . . C6 C 0.5937 0.2604 0.0833 0.150(8) Uiso 0.30 2 d SP . . C7 C 0.5883 0.2502 0.1538 0.147(10) Uiso 0.16 1 d P . . C8 C 0.6360 0.4007 0.3027 0.069(10) Uiso 0.06 1 d P . . 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 S1 0.0731(6) 0.0860(7) 0.0241(5) -0.0043(3) -0.00215(14) 0.0430(4) N1 0.0930(16) 0.131(2) 0.0340(9) 0.0022(10) 0.0035(9) 0.0737(16) C1 0.0700(15) 0.077(2) 0.0271(12) 0.0025(12) 0.0012(6) 0.0386(10) _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 S1 C1 1.708(4) . ? N1 C1 1.321(3) . ? N1 H1A 0.8800 . ? N1 H1B 0.8800 . ? C1 N1 1.321(3) 4 ? C2 C8 1.0881 33_545 ? C2 C3 1.1804 . ? C2 C8 1.3576 2_655 ? C2 C4 1.4149 . ? C2 C8 1.4680 . ? C2 C3 1.7101 3_665 ? C2 C4 1.8017 31_655 ? C2 C7 1.8151 . ? C2 C2 1.9785 32 ? C2 C2 1.9786 33_545 ? C2 C3 1.9999 2_655 ? C3 C3 0.9420 3_665 ? C3 C3 0.9420 2_655 ? C3 C7 1.1084 . ? C3 C4 1.1375 . ? C3 C8 1.4243 2_655 ? C3 C7 1.6792 3_665 ? C3 C2 1.7101 2_655 ? C3 C5 1.7623 . ? C3 C8 1.7864 . ? C3 C6 1.7922 . ? C3 C7 1.8879 2_655 ? C4 C4 0.8838 31_655 ? C4 C3 1.1375 2_655 ? C4 C3 1.1375 3_665 ? C4 C8 1.3624 3_665 ? C4 C8 1.3624 2_655 ? C4 C8 1.3624 . ? C4 C2 1.4149 2_655 ? C4 C2 1.4149 3_665 ? C4 C8 1.5909 33_545 ? C4 C8 1.5910 32 ? C5 C6 1.1427 2_655 ? C5 C6 1.1427 . ? C5 C6 1.1427 3_665 ? C5 C7 1.5412 16_554 ? C5 C7 1.5413 2_655 ? C5 C7 1.5413 . ? C5 C7 1.5413 3_665 ? C5 C7 1.5413 18_544 ? C5 C7 1.5413 17_654 ? C5 C3 1.7623 2_655 ? C5 C3 1.7623 3_665 ? C6 C7 0.8889 . ? C6 C7 0.8889 18_544 ? C6 C3 1.7923 18_544 ? C6 C6 1.9792 3_665 ? C6 C6 1.9792 2_655 ? C7 C3 1.6792 2_655 ? C7 C7 1.7609 18_544 ? C7 C3 1.8879 3_665 ? C7 C8 1.8904 2_655 ? C8 C2 1.0881 32 ? C8 C2 1.3576 3_665 ? C8 C3 1.4243 3_665 ? C8 C8 1.5608 33_545 ? C8 C8 1.5608 32 ? C8 C4 1.5910 31_655 ? C8 C7 1.8904 3_665 ? C8 C3 2.0376 32 ? 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 N1 H1A 120.0 . . ? C1 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? N1 C1 N1 118.9(3) 4 . ? N1 C1 S1 120.57(16) 4 . ? N1 C1 S1 120.57(16) . . ? C8 C2 C3 127.792(2) 33_545 . ? C8 C2 C8 78.455(1) 33_545 2_655 ? C3 C2 C8 67.860(1) . 2_655 ? C8 C2 C4 77.7 33_545 . ? C3 C2 C4 51.015(2) . . ? C8 C2 C4 58.8 2_655 . ? C8 C2 C8 73.584(1) 33_545 . ? C3 C2 C8 84.085(1) . . ? C8 C2 C8 113.0 2_655 . ? C4 C2 C8 56.4 . . ? C8 C2 C3 112.784(1) 33_545 3_665 ? C3 C2 C3 31.8 . 3_665 ? C8 C2 C3 87.799(1) 2_655 3_665 ? C4 C2 C3 41.355(2) . 3_665 ? C8 C2 C3 52.582(1) . 3_665 ? C8 C2 C4 48.969(2) 33_545 31_655 ? C3 C2 C4 79.178(3) . 31_655 ? C8 C2 C4 58.5 2_655 31_655 ? C4 C2 C4 28.819(1) . 31_655 ? C8 C2 C4 57.1 . 31_655 ? C3 C2 C4 67.786(3) 3_665 31_655 ? C8 C2 C7 149.870(1) 33_545 . ? C3 C2 C7 36.165(1) . . ? C8 C2 C7 71.494(2) 2_655 . ? C4 C2 C7 84.842(1) . . ? C8 C2 C7 116.3 . . ? C3 C2 C7 64.683(1) 3_665 . ? C4 C2 C7 110.139(2) 31_655 . ? C8 C2 C2 40.882(1) 33_545 32 ? C3 C2 C2 107.042(2) . 32 ? C8 C2 C2 100.090(1) 2_655 32 ? C4 C2 C2 61.5 . 32 ? C8 C2 C2 32.749(1) . 32 ? C3 C2 C2 79.464(2) 3_665 32 ? C4 C2 C2 43.649(1) 31_655 32 ? C7 C2 C2 143.141(1) . 32 ? C8 C2 C2 46.869(1) 33_545 33_545 ? C3 C2 C2 93.604(3) . 33_545 ? C8 C2 C2 31.637(1) 2_655 33_545 ? C4 C2 C2 61.5 . 33_545 ? C8 C2 C2 99.326(1) . 33_545 ? C3 C2 C2 101.671(2) 3_665 33_545 ? C4 C2 C2 43.648(1) 31_655 33_545 ? C7 C2 C2 103.129(3) . 33_545 ? C2 C2 C2 74.979(2) 32 33_545 ? C8 C2 C3 110.559(1) 33_545 2_655 ? C3 C2 C3 17.4 . 2_655 ? C8 C2 C3 60.771(1) 2_655 2_655 ? C4 C2 C3 33.711(2) . 2_655 ? C8 C2 C3 74.537(1) . 2_655 ? C3 C2 C3 28.0 3_665 2_655 ? C4 C2 C3 61.803(3) 31_655 2_655 ? C7 C2 C3 52.0 . 2_655 ? C2 C2 C3 92.126(2) 32 2_655 ? C2 C2 C3 81.004(2) 33_545 2_655 ? C3 C3 C3 60.0 3_665 2_655 ? C3 C3 C7 133.924(1) 3_665 . ? C3 C3 C7 109.702(1) 2_655 . ? C3 C3 C4 65.540(1) 3_665 . ? C3 C3 C4 65.540(1) 2_655 . ? C7 C3 C4 156.503(1) . . ? C3 C3 C2 106.824(1) 3_665 . ? C3 C3 C2 140.621(2) 2_655 . ? C7 C3 C2 104.898(2) . . ? C4 C3 C2 75.214(3) . . ? C3 C3 C8 128.577(1) 3_665 2_655 ? C3 C3 C8 95.9 2_655 2_655 ? C7 C3 C8 95.750(3) . 2_655 ? C4 C3 C8 63.091(2) . 2_655 ? C2 C3 C8 61.995(2) . 2_655 ? C3 C3 C7 38.419(1) 3_665 3_665 ? C3 C3 C7 87.4 2_655 3_665 ? C7 C3 C7 101.868(2) . 3_665 ? C4 C3 C7 100.881(2) . 3_665 ? C2 C3 C7 103.490(1) . 3_665 ? C8 C3 C7 159.8 2_655 3_665 ? C3 C3 C2 93.3 3_665 2_655 ? C3 C3 C2 41.355(1) 2_655 2_655 ? C7 C3 C2 105.062(1) . 2_655 ? C4 C3 C2 55.270(1) . 2_655 ? C2 C3 C2 111.539(2) . 2_655 ? C8 C3 C2 54.943(1) 2_655 2_655 ? C7 C3 C2 127.662(1) 3_665 2_655 ? C3 C3 C5 74.499(1) 3_665 . ? C3 C3 C5 74.498(1) 2_655 . ? C7 C3 C5 59.910(2) . . ? C4 C3 C5 133.462(2) . . ? C2 C3 C5 141.563(1) . . ? C8 C3 C5 146.783(1) 2_655 . ? C7 C3 C5 53.145(1) 3_665 . ? C2 C3 C5 106.658(2) 2_655 . ? C3 C3 C8 52.476(1) 3_665 . ? C3 C3 C8 98.7 2_655 . ? C7 C3 C8 148.800(1) . . ? C4 C3 C8 49.692(1) . . ? C2 C3 C8 54.823(1) . . ? C8 C3 C8 93.803(3) 2_655 . ? C7 C3 C8 66.028(3) 3_665 . ? C2 C3 C8 104.739(2) 2_655 . ? C5 C3 C8 118.841(2) . . ? C3 C3 C6 110.716(1) 3_665 . ? C3 C3 C6 100.7 2_655 . ? C7 C3 C6 23.243(1) . . ? C4 C3 C6 166.045(1) . . ? C2 C3 C6 118.288(2) . . ? C8 C3 C6 118.515(2) 2_655 . ? C7 C3 C6 80.112(2) 3_665 . ? C2 C3 C6 113.090(1) 2_655 . ? C5 C3 C6 37.492(2) . . ? C8 C3 C6 139.841(1) . . ? C3 C3 C7 62.690(1) 3_665 2_655 ? C3 C3 C7 25.015(1) 2_655 2_655 ? C7 C3 C7 90.287(2) . 2_655 ? C4 C3 C7 89.687(2) . 2_655 ? C2 C3 C7 164.5 . 2_655 ? C8 C3 C7 114.310(1) 2_655 2_655 ? C7 C3 C7 75.661(1) 3_665 2_655 ? C2 C3 C7 60.352(2) 2_655 2_655 ? C5 C3 C7 49.8 . 2_655 ? C8 C3 C7 112.515(1) . 2_655 ? C6 C3 C7 77.011(2) . 2_655 ? C4 C4 C3 151.435(1) 31_655 2_655 ? C4 C4 C3 151.438(1) 31_655 . ? C3 C4 C3 48.920(2) 2_655 . ? C4 C4 C3 151.440(1) 31_655 3_665 ? C3 C4 C3 48.920(2) 2_655 3_665 ? C3 C4 C3 48.920(2) . 3_665 ? C4 C4 C8 87.5 31_655 3_665 ? C3 C4 C8 68.791(1) 2_655 3_665 ? C3 C4 C8 117.670(1) . 3_665 ? C3 C4 C8 90.8 3_665 3_665 ? C4 C4 C8 87.5 31_655 2_655 ? C3 C4 C8 90.8 2_655 2_655 ? C3 C4 C8 68.790(1) . 2_655 ? C3 C4 C8 117.670(1) 3_665 2_655 ? C8 C4 C8 119.8 3_665 2_655 ? C4 C4 C8 87.5 31_655 . ? C3 C4 C8 117.669(1) 2_655 . ? C3 C4 C8 90.8 . . ? C3 C4 C8 68.790(1) 3_665 . ? C8 C4 C8 119.8 3_665 . ? C8 C4 C8 119.8 2_655 . ? C4 C4 C2 100.7 31_655 2_655 ? C3 C4 C2 53.771(1) 2_655 2_655 ? C3 C4 C2 83.375(1) . 2_655 ? C3 C4 C2 102.632(1) 3_665 2_655 ? C8 C4 C2 58.5 3_665 2_655 ? C8 C4 C2 63.8 2_655 2_655 ? C8 C4 C2 171.4 . 2_655 ? C4 C4 C2 100.668(1) 31_655 3_665 ? C3 C4 C2 83.374(1) 2_655 3_665 ? C3 C4 C2 102.631(1) . 3_665 ? C3 C4 C2 53.771(1) 3_665 3_665 ? C8 C4 C2 63.8 3_665 3_665 ? C8 C4 C2 171.4 2_655 3_665 ? C8 C4 C2 58.5 . 3_665 ? C2 C4 C2 116.7 2_655 3_665 ? C4 C4 C2 100.669(1) 31_655 . ? C3 C4 C2 102.631(1) 2_655 . ? C3 C4 C2 53.770(1) . . ? C3 C4 C2 83.374(1) 3_665 . ? C8 C4 C2 171.4 3_665 . ? C8 C4 C2 58.5 2_655 . ? C8 C4 C2 63.8 . . ? C2 C4 C2 116.7 2_655 . ? C2 C4 C2 116.7 3_665 . ? C4 C4 C8 58.816(1) 31_655 33_545 ? C3 C4 C8 142.909(1) 2_655 33_545 ? C3 C4 C8 95.177(3) . 33_545 ? C3 C4 C8 118.456(1) 3_665 33_545 ? C8 C4 C8 146.292(1) 3_665 33_545 ? C8 C4 C8 63.2 2_655 33_545 ? C8 C4 C8 63.3 . 33_545 ? C2 C4 C8 123.4 2_655 33_545 ? C2 C4 C8 118.8 3_665 33_545 ? C2 C4 C8 41.935(2) . 33_545 ? C4 C4 C8 58.815(1) 31_655 32 ? C3 C4 C8 118.454(2) 2_655 32 ? C3 C4 C8 142.9 . 32 ? C3 C4 C8 95.177(2) 3_665 32 ? C8 C4 C8 63.2 3_665 32 ? C8 C4 C8 146.293(1) 2_655 32 ? C8 C4 C8 63.3 . 32 ? C2 C4 C8 118.8 2_655 32 ? C2 C4 C8 41.935(2) 3_665 32 ? C2 C4 C8 123.4 . 32 ? C8 C4 C8 95.615(2) 33_545 32 ? C6 C5 C6 120.0 2_655 . ? C6 C5 C6 120.0 2_655 3_665 ? C6 C5 C6 120.0 . 3_665 ? C6 C5 C7 111.9 2_655 16_554 ? C6 C5 C7 116.6 . 16_554 ? C6 C5 C7 34.839(1) 3_665 16_554 ? C6 C5 C7 34.837(1) 2_655 2_655 ? C6 C5 C7 116.5 . 2_655 ? C6 C5 C7 112.0 3_665 2_655 ? C7 C5 C7 126.902(1) 16_554 2_655 ? C6 C5 C7 112.0 2_655 . ? C6 C5 C7 34.836(1) . . ? C6 C5 C7 116.544(1) 3_665 . ? C7 C5 C7 136.098(1) 16_554 . ? C7 C5 C7 90.756(2) 2_655 . ? C6 C5 C7 116.5 2_655 3_665 ? C6 C5 C7 112.0 . 3_665 ? C6 C5 C7 34.836(1) 3_665 3_665 ? C7 C5 C7 69.676(3) 16_554 3_665 ? C7 C5 C7 90.756(2) 2_655 3_665 ? C7 C5 C7 90.756(2) . 3_665 ? C6 C5 C7 116.6 2_655 18_544 ? C6 C5 C7 34.838(1) . 18_544 ? C6 C5 C7 111.949(1) 3_665 18_544 ? C7 C5 C7 90.757(2) 16_554 18_544 ? C7 C5 C7 136.095(1) 2_655 18_544 ? C7 C5 C7 69.674(3) . 18_544 ? C7 C5 C7 126.905(1) 3_665 18_544 ? C6 C5 C7 34.837(1) 2_655 17_654 ? C6 C5 C7 111.9 . 17_654 ? C6 C5 C7 116.554(1) 3_665 17_654 ? C7 C5 C7 90.755(2) 16_554 17_654 ? C7 C5 C7 69.674(3) 2_655 17_654 ? C7 C5 C7 126.902(1) . 17_654 ? C7 C5 C7 136.098(1) 3_665 17_654 ? C7 C5 C7 90.754(2) 18_544 17_654 ? C6 C5 C3 72.677(1) 2_655 2_655 ? C6 C5 C3 94.5 . 2_655 ? C6 C5 C3 102.658(1) 3_665 2_655 ? C7 C5 C3 135.443(1) 16_554 2_655 ? C7 C5 C3 38.478(1) 2_655 2_655 ? C7 C5 C3 60.665(2) . 2_655 ? C7 C5 C3 69.338(2) 3_665 2_655 ? C7 C5 C3 128.245(1) 18_544 2_655 ? C7 C5 C3 107.100(2) 17_654 2_655 ? C6 C5 C3 94.5 2_655 3_665 ? C6 C5 C3 102.658(1) . 3_665 ? C6 C5 C3 72.677(1) 3_665 3_665 ? C7 C5 C3 107.102(2) 16_554 3_665 ? C7 C5 C3 60.665(2) 2_655 3_665 ? C7 C5 C3 69.338(2) . 3_665 ? C7 C5 C3 38.478(1) 3_665 3_665 ? C7 C5 C3 135.443(1) 18_544 3_665 ? C7 C5 C3 128.246(1) 17_654 3_665 ? C3 C5 C3 31.003(1) 2_655 3_665 ? C6 C5 C3 102.658(1) 2_655 . ? C6 C5 C3 72.677(1) . . ? C6 C5 C3 94.5 3_665 . ? C7 C5 C3 128.247(1) 16_554 . ? C7 C5 C3 69.338(2) 2_655 . ? C7 C5 C3 38.478(1) . . ? C7 C5 C3 60.665(2) 3_665 . ? C7 C5 C3 107.101(2) 18_544 . ? C7 C5 C3 135.441(1) 17_654 . ? C3 C5 C3 31.003(1) 2_655 . ? C3 C5 C3 31.003(1) 3_665 . ? C7 C6 C7 164.176(1) . 18_544 ? C7 C6 C5 97.912(1) . . ? C7 C6 C5 97.9 18_544 . ? C7 C6 C3 29.476(1) . . ? C7 C6 C3 164.896(1) 18_544 . ? C5 C6 C3 69.831(1) . . ? C7 C6 C3 164.905(1) . 18_544 ? C7 C6 C3 29.477(1) 18_544 18_544 ? C5 C6 C3 69.832(1) . 18_544 ? C3 C6 C3 139.662(2) . 18_544 ? C7 C6 C6 98.961(1) . 3_665 ? C7 C6 C6 94.7 18_544 3_665 ? C5 C6 C6 30.0 . 3_665 ? C3 C6 C6 70.215(1) . 3_665 ? C3 C6 C6 75.006(1) 18_544 3_665 ? C7 C6 C6 94.7 . 2_655 ? C7 C6 C6 99.0 18_544 2_655 ? C5 C6 C6 30.0 . 2_655 ? C3 C6 C6 75.006(1) . 2_655 ? C3 C6 C6 70.217(1) 18_544 2_655 ? C6 C6 C6 60.0 3_665 2_655 ? C6 C7 C3 127.281(2) . . ? C6 C7 C5 47.251(1) . . ? C3 C7 C5 81.612(3) . . ? C6 C7 C3 111.996(2) . 2_655 ? C3 C7 C3 31.9 . 2_655 ? C5 C7 C3 66.190(2) . 2_655 ? C6 C7 C7 7.9 . 18_544 ? C3 C7 C7 134.777(2) . 18_544 ? C5 C7 C7 55.163(1) . 18_544 ? C3 C7 C7 119.625(1) 2_655 18_544 ? C6 C7 C2 141.518(2) . . ? C3 C7 C2 38.938(1) . . ? C5 C7 C2 111.909(2) . . ? C3 C7 C2 69.702(1) 2_655 . ? C7 C7 C2 143.606(2) 18_544 . ? C6 C7 C3 106.254(2) . 3_665 ? C3 C7 C3 21.1 . 3_665 ? C5 C7 C3 60.856(2) . 3_665 ? C3 C7 C3 29.9 2_655 3_665 ? C7 C7 C3 113.835(1) 18_544 3_665 ? C2 C7 C3 54.965(1) . 3_665 ? C6 C7 C8 170.498(1) . 2_655 ? C3 C7 C8 48.562(2) . 2_655 ? C5 C7 C8 125.515(1) . 2_655 ? C3 C7 C8 59.712(1) 2_655 2_655 ? C7 C7 C8 173.5 18_544 2_655 ? C2 C7 C8 42.926(2) . 2_655 ? C3 C7 C8 69.081(1) 3_665 2_655 ? C2 C8 C2 107.5 32 3_665 ? C2 C8 C4 94.0 32 . ? C2 C8 C4 62.7 3_665 . ? C2 C8 C3 140.421(2) 32 3_665 ? C2 C8 C3 50.1 3_665 3_665 ? C4 C8 C3 48.119(1) . 3_665 ? C2 C8 C2 100.380(1) 32 . ? C2 C8 C2 116.9 3_665 . ? C4 C8 C2 59.8 . . ? C3 C8 C2 72.5 3_665 . ? C2 C8 C8 58.458(1) 32 33_545 ? C2 C8 C8 124.8 3_665 33_545 ? C4 C8 C8 65.5 . 33_545 ? C3 C8 C8 104.122(2) 3_665 33_545 ? C2 C8 C8 41.968(2) . 33_545 ? C2 C8 C8 64.447(2) 32 32 ? C2 C8 C8 43.082(2) 3_665 32 ? C4 C8 C8 65.537(1) . 32 ? C3 C8 C8 85.961(3) 3_665 32 ? C2 C8 C8 121.9 . 32 ? C8 C8 C8 98.085(2) 33_545 32 ? C2 C8 C4 60.340(1) 32 31_655 ? C2 C8 C4 74.856(1) 3_665 31_655 ? C4 C8 C4 33.706(2) . 31_655 ? C3 C8 C4 80.869(3) 3_665 31_655 ? C2 C8 C4 72.041(1) . 31_655 ? C8 C8 C4 51.210(1) 33_545 31_655 ? C8 C8 C4 51.210(1) 32 31_655 ? C2 C8 C3 126.303(2) 32 . ? C2 C8 C3 77.683(1) 3_665 . ? C4 C8 C3 39.546(1) . . ? C3 C8 C3 31.636(1) 3_665 . ? C2 C8 C3 41.1 . . ? C8 C8 C3 74.654(2) 33_545 . ? C8 C8 C3 101.217(2) 32 . ? C4 C8 C3 70.667(3) 31_655 . ? C2 C8 C7 173.0 32 3_665 ? C2 C8 C7 65.6 3_665 3_665 ? C4 C8 C7 83.4 . 3_665 ? C3 C8 C7 35.688(1) 3_665 3_665 ? C2 C8 C7 83.893(1) . 3_665 ? C8 C8 C7 125.386(1) 33_545 3_665 ? C8 C8 C7 108.634(2) 32 3_665 ? C4 C8 C7 116.542(2) 31_655 3_665 ? C3 C8 C7 54.261(1) . 3_665 ? C2 C8 C3 27.243(1) 32 32 ? C2 C8 C3 97.082(1) 3_665 32 ? C4 C8 C3 67.024(1) . 32 ? C3 C8 C3 114.647(3) 3_665 32 ? C2 C8 C3 83.233(1) . 32 ? C8 C8 C3 44.210(1) 33_545 32 ? C8 C8 C3 57.723(1) 32 32 ? C4 C8 C3 33.8 31_655 32 ? C3 C8 C3 99.950(3) . 32 ? C7 C8 C3 150.300(1) 3_665 32 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.452 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.042