#------------------------------------------------------------------------------ #$Date: 2012-02-26 23:34:47 +0200 (Sun, 26 Feb 2012) $ #$Revision: 35909 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/56/7205693.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_7205693 loop_ _publ_author_name 'Lenthall, Joseph T.' 'Foster, Jonathan A.' 'Anderson, Kirsty M.' 'Probert, Michael R.' 'Howard, Judith A. K.' 'Steed, Jonathan W.' _publ_section_title ; Hydrogen bonding interactions with the thiocarbonyl \p-system ; _journal_issue 9 _journal_name_full CrystEngComm _journal_page_first 3202 _journal_volume 13 _journal_year 2011 _chemical_formula_moiety 'C6 H14 N4 S2' _chemical_formula_sum 'C6 H14 N4 S2' _chemical_formula_weight 206.33 _chemical_name_systematic ; ? ; _space_group_crystal_system tetragonal _space_group_IT_number 86 _space_group_name_Hall '-P 4bc' _space_group_name_H-M_alt 'P 42/n' _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4bc' _symmetry_space_group_name_H-M 'P 42/n :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2010-09-28 _audit_creation_method ; Olex2 1.1-beta (compiled 2010.09.10 svn.r1414, GUI svn.r3225) ; _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.5098(5) _cell_length_b 9.5098(5) _cell_length_c 10.8333(7) _cell_measurement_reflns_used 1455 _cell_measurement_temperature 200 _cell_measurement_theta_max 26.83 _cell_measurement_theta_min 2.85 _cell_volume 979.72(10) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'SMART v5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)/Bruker' _diffrn_ambient_temperature 200 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.6 _diffrn_detector_type 'Bruker SMART CCD 6000 area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.038066 _diffrn_orient_matrix_UB_12 -0.067548 _diffrn_orient_matrix_UB_13 0.062351 _diffrn_orient_matrix_UB_21 -0.062970 _diffrn_orient_matrix_UB_22 0.041643 _diffrn_orient_matrix_UB_23 0.064283 _diffrn_orient_matrix_UB_31 -0.075092 _diffrn_orient_matrix_UB_32 -0.069024 _diffrn_orient_matrix_UB_33 -0.022240 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 6601 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.85 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 35.0 _diffrn_source_power 1.75 _diffrn_source_target Mo _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 0.498 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.399 _exptl_crystal_description block _exptl_crystal_F_000 440 _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.209 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 56 _refine_ls_number_reflns 1002 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.921 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0296 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.0685 _reflns_number_gt 716 _reflns_number_total 1002 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0ce00680g.txt _[local]_cod_data_source_block jws1 _[local]_cod_cif_authors_sg_H-M P4(2)/n _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_database_code 7205693 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y, x+1/2, z+1/2' 3 '-x+1/2, -y+1/2, z' 4 'y+1/2, -x, z+1/2' 5 '-x, -y, -z' 6 'y, -x-1/2, -z-1/2' 7 'x-1/2, y-1/2, -z' 8 '-y-1/2, x, -z-1/2' 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 0.10525(5) 0.47966(5) 0.17890(4) 0.02688(16) Uani 1 1 d . . . N2 N 0.09555(15) 0.74683(15) 0.25753(13) 0.0213(3) Uani 1 1 d . . . H2 H 0.0679 0.8344 0.2479 0.026 Uiso 1 1 calc R . . C2 C 0.05801(18) 0.65297(18) 0.17119(16) 0.0200(4) Uani 1 1 d . . . N1 N -0.02338(15) 0.69749(15) 0.07867(14) 0.0231(4) Uani 1 1 d . . . H1 H -0.0431 0.6367 0.0199 0.028 Uiso 1 1 calc R . . C1 C -0.0820(2) 0.83771(19) 0.06699(18) 0.0284(5) Uani 1 1 d . . . H1A H -0.1246 0.8484 -0.0148 0.043 Uiso 1 1 calc R . . H1C H -0.0070 0.9075 0.0773 0.043 Uiso 1 1 calc R . . H1B H -0.1538 0.8520 0.1306 0.043 Uiso 1 1 calc R . . C3 C 0.17901(19) 0.71320(19) 0.36599(16) 0.0228(4) Uani 1 1 d . . . H3A H 0.1940 0.6103 0.3695 0.027 Uiso 1 1 calc R . . H3B H 0.1262 0.7410 0.4409 0.027 Uiso 1 1 calc 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 S1 0.0336(3) 0.0201(3) 0.0270(3) -0.0036(2) -0.0051(2) 0.0053(2) N2 0.0237(8) 0.0179(8) 0.0223(8) 0.0009(7) -0.0016(7) -0.0011(6) C2 0.0156(8) 0.0222(9) 0.0221(10) -0.0008(8) 0.0059(8) -0.0022(7) N1 0.0274(8) 0.0202(8) 0.0218(9) -0.0042(7) -0.0050(7) 0.0036(6) C1 0.0310(11) 0.0237(10) 0.0305(11) -0.0002(9) -0.0030(9) 0.0068(8) C3 0.0268(10) 0.0249(10) 0.0166(9) 0.0020(8) 0.0018(8) -0.0043(8) 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' 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 N2 C2 S1 122.50(14) . . ? N2 C3 C3 112.55(12) . 3_565 ? C2 N2 C3 124.24(16) . . ? C2 N1 C1 125.41(15) . . ? N1 C2 S1 119.63(13) . . ? N1 C2 N2 117.82(16) . . ? 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 C2 1.7103(18) . ? N2 C2 1.341(2) . ? N2 C3 1.454(2) . ? C2 N1 1.335(2) . ? N1 C1 1.451(2) . ? C3 C3 1.521(3) 3_565 ?