#------------------------------------------------------------------------------ #$Date: 2016-02-16 20:30:59 +0000 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/06/4000687.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000687 loop_ _publ_author_name 'Thierry Maris' 'Michael J. Henson' 'Stephen J. Heyes' 'Keith Prout' _publ_section_title ; Investigations of the Phase Transitions in Thiourea Inclusion Compounds with Cycloheptane, Cyclooctane, and Cyclooctanone ; _journal_name_full 'Chem. Mater.' _journal_page_first 2483 _journal_page_last 2492 _journal_paper_doi 10.1021/cm991173u _journal_volume 13 _journal_year 2001 _chemical_formula_sum 'C11 H28 N6 S3' _chemical_formula_weight 54.07 _space_group_IT_number 167 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-R 3 2"c' _symmetry_space_group_name_H-M 'R -3 c :H' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 16.225(2) _cell_length_b 16.225(2) _cell_length_c 12.488(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 19 _cell_measurement_theta_min 8 _cell_volume 2847.0(10) _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_max 0.967 _diffrn_measurement_method \w/2\q _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 1309 _diffrn_reflns_theta_max 78.00 _diffrn_reflns_theta_min 0.00 _diffrn_standards_decay_% 32.38 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 3.52 _exptl_absorpt_correction_T_max 0.51 _exptl_absorpt_correction_T_min 0.41 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '\y scan,(North et al, 1968)' _exptl_crystal_colour ' colourless ' _exptl_crystal_density_diffrn 1.14 _exptl_crystal_description ' block ' _exptl_crystal_F_000 1015.72 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _refine_diff_density_max 1.07 _refine_diff_density_min -0.91 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.9657 _refine_ls_number_parameters 22 _refine_ls_number_reflns 923 _refine_ls_R_factor_gt 0.0922 _refine_ls_shift/su_max 0.000538 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 7.99 7.52 5.75 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1091 _reflns_limit_h_max 0 _reflns_limit_h_min -17 _reflns_limit_k_max 20 _reflns_limit_k_min 0 _reflns_limit_l_max 15 _reflns_limit_l_min -14 _reflns_number_gt 923 _reflns_number_total 1309 _reflns_threshold_expression >3.00\s(I) _cod_data_source_file deposit.cif _cod_data_source_block TC8 _cod_original_cell_volume 2847.0 _cod_original_sg_symbol_H-M R-3c _cod_original_formula_sum ' C1.83 H2 N1 S0.50 ' _cod_database_code 4000687 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/3,y+2/3,z+2/3 -x+1/3,-y+2/3,-z+2/3 x+2/3,y+1/3,z+1/3 -x+2/3,-y+1/3,-z+1/3 -y,x-y,z y,-x+y,-z -y+1/3,x-y+2/3,z+2/3 y+1/3,-x+y+2/3,-z+2/3 -y+2/3,x-y+1/3,z+1/3 y+2/3,-x+y+1/3,-z+1/3 -x+y,-x,z x-y,x,-z -x+y+1/3,-x+2/3,z+2/3 x-y+1/3,x+2/3,-z+2/3 -x+y+2/3,-x+1/3,z+1/3 x-y+2/3,x+1/3,-z+1/3 -x+y,y,z+1/2 x-y,-y,-z+1/2 -x+y+1/3,y+2/3,z+7/6 x-y+1/3,-y+2/3,-z+7/6 -x+y+2/3,y+1/3,z+5/6 x-y+2/3,-y+1/3,-z+5/6 x,x-y,z+1/2 -x,-x+y,-z+1/2 x+1/3,x-y+2/3,z+7/6 -x+1/3,-x+y+2/3,-z+7/6 x+2/3,x-y+1/3,z+5/6 -x+2/3,-x+y+1/3,-z+5/6 -y,-x,z+1/2 y,x,-z+1/2 -y+1/3,-x+2/3,z+7/6 y+1/3,x+2/3,-z+7/6 -y+2/3,-x+1/3,z+5/6 y+2/3,x+1/3,-z+5/6 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type S1 0.69527(5) 0.0000 0.2500 0.0851 1.0000 Uani C2 0.5908(2) 0.0000 0.2500 0.0804 1.0000 Uani N3 0.53932(18) -0.0184(2) 0.16083(18) 0.0962 1.0000 Uani C4 0.3333 0.6667 -0.0833 0.109(3) 8.0000 Uiso H1 0.5566 -0.0318 0.0906 0.0500 1.0000 Uiso H2 0.4750 -0.0169 0.1654 0.0500 1.0000 Uiso 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 0.0985(6) 0.1144(7) 0.0478(6) -0.0028(3) -0.00141(17) 0.0572(4) C2 0.0940(15) 0.094(2) 0.0535(18) 0.0009(14) 0.0004(7) 0.0468(11) N3 0.1032(16) 0.128(2) 0.0595(12) -0.002(1) -0.008(1) 0.0594(15) C4 0.109(3) 1.859(8) 0.0000 0.0000 0.0000 0.0000 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 C2 N3 . 120.96(17) yes S1 C2 N3 20_555 120.96(17) yes N3 C2 N3 20_555 118.1(3) yes C2 N3 H1 . 125.6(2) no C2 N3 H2 . 117.7(2) no H1 N3 H2 . 116.7(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C2 . 1.695(4) yes C2 N3 . 1.333(3) yes C2 N3 20_555 1.333(3) yes N3 H1 . 0.977(2) no N3 H2 . 1.057(2) no