#------------------------------------------------------------------------------ #$Date: 2016-02-16 20:30:59 +0000 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/06/4000685.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_4000685 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 'C10 H26 N6 S3' _chemical_formula_weight 52.07 _chemical_name_systematic ; ? ; _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 99-19-07 _audit_creation_method CRYSTALS_ver_12-03-99 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 16.012(2) _cell_length_b 16.012(2) _cell_length_c 12.447(2) _cell_measurement_reflns_used 15 _cell_measurement_temperature 293 _cell_measurement_theta_max 23 _cell_measurement_theta_min 22 _cell_volume 2763.7(7) _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction ; RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_max 0.527 _diffrn_measurement_device_type ' Enraf-nonius CAD4 ' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_reflns_av_R_equivalents 0.03 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 743 _diffrn_reflns_theta_max 75.00 _diffrn_reflns_theta_min 0.00 _diffrn_standards_decay_% 0.00 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.66 _exptl_absorpt_correction_T_max 0.48 _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '\y scan,(North et al, 1968)' _exptl_crystal_colour ' colourless ' _exptl_crystal_density_diffrn 1.13 _exptl_crystal_description ' prism ' _exptl_crystal_F_000 979.62 _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.51 _refine_diff_density_min -0.59 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.8824 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 22 _refine_ls_number_reflns 524 _refine_ls_R_factor_gt 0.0827 _refine_ls_shift/su_max 0.000128 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 12.1 9.42 9.15 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1078 _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 -5 _reflns_number_gt 524 _reflns_number_total 667 _reflns_threshold_expression >3.00\s(I) _cod_data_source_file deposit.cif _cod_data_source_block TC7_RT _cod_original_cell_volume 2763.8 _cod_original_sg_symbol_H-M R-3c _cod_original_formula_sum ' C1.67 H2 N1 S0.50 ' _cod_database_code 4000685 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 0.69782(7) 0.0000 0.2500 0.0727 1.0000 Uani C2 0.5908(3) 0.0000 0.2500 0.0695 1.0000 Uani N3 0.5403(2) -0.0178(3) 0.1614(2) 0.0852 1.0000 Uani C4 0.3333 0.6667 -0.0833 0.103(5) 7.0000 Uiso H31 0.5612 -0.0334 0.0913 0.0944 1.0000 Uiso H32 0.4746 -0.0191 0.1590 0.0944 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 0.0798(7) 0.0940(9) 0.0490(8) -0.0044(4) -0.0022(2) 0.0470(4) C2 0.0756(18) 0.079(2) 0.055(2) 0.0030(17) 0.0015(9) 0.0397(12) N3 0.0877(18) 0.113(2) 0.0613(16) -0.0022(14) -0.0066(13) 0.0548(17) C4 0.103(5) 1.676(11) 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 . 120.5(2) yes S1 C2 N3 20_555 120.5(2) yes N3 C2 N3 20_555 118.9(4) yes C2 N3 H31 . 122.4(3) no C2 N3 H32 . 122.3(3) no H31 N3 H32 . 115.3(3) 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 . 1.713(5) yes C2 N3 . 1.313(4) yes C2 N3 20_555 1.313(4) yes N3 H31 . 1.009(3) no N3 H32 . 1.042(3) no