#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/48/2204871.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2204871 loop_ _publ_author_name 'Liang-zhong Xu' 'Hai-Zhen Xu' 'Shuang-Hua Yang' 'Chun-Li Li' 'Kai Zhou' _publ_section_title ; 1,2-Bis(1,3-dithiolan-2-ylidene)hydrazine ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o31 _journal_page_last o32 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac 'C6 H8 N2 S4' _chemical_formula_moiety 'C6 H8 N2 S4' _chemical_formula_sum 'C6 H8 N2 S4' _chemical_formula_weight 236.38 _chemical_name_systematic ; 1,2-Bis(1,3-dithiolan-2-ylidene)hydrazine ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 106.712(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.300(2) _cell_length_b 7.737(2) _cell_length_c 10.386(3) _cell_measurement_reflns_used 1494 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.37 _cell_measurement_theta_min 2.63 _cell_volume 484.9(2) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1999)' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2712 _diffrn_reflns_theta_full 26.38 _diffrn_reflns_theta_max 26.38 _diffrn_reflns_theta_min 3.34 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_correction_T_min 0.867242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_meas NONE _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 244 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _refine_diff_density_max 1.057 _refine_diff_density_min -0.367 _refine_ls_extinction_coef 0.161(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 56 _refine_ls_number_reflns 992 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0456 _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^)+(0.0675P)^2^+0.6306P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1202 _refine_ls_wR_factor_ref 0.1304 _reflns_number_gt 834 _reflns_number_total 992 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cv6424.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2204871 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol S1 1.10441(14) 0.27867(12) 0.15937(10) 0.0489(4) Uani d . 1 S S2 0.61750(14) 0.25208(11) 0.04382(9) 0.0483(4) Uani d . 1 S N1 0.8901(4) 0.0247(4) -0.0092(3) 0.0449(7) Uani d . 1 N C1 0.8784(5) 0.1649(4) 0.0550(3) 0.0363(7) Uani d . 1 C C2 0.9419(6) 0.4598(4) 0.1896(4) 0.0506(8) Uani d . 1 C H2A 1.0134 0.5113 0.2764 0.061 Uiso calc R 1 H H2B 0.9290 0.5473 0.1208 0.061 Uiso calc R 1 H C3 0.7157(5) 0.3936(4) 0.1865(3) 0.0459(8) Uani d . 1 C H3A 0.6141 0.4897 0.1795 0.055 Uiso calc R 1 H H3B 0.7239 0.3312 0.2688 0.055 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0380(5) 0.0475(6) 0.0583(6) 0.0010(3) 0.0093(4) -0.0102(4) S2 0.0400(5) 0.0539(6) 0.0475(6) 0.0052(3) 0.0069(4) -0.0102(3) N1 0.0362(14) 0.0474(15) 0.0490(15) 0.0021(11) 0.0089(11) -0.0090(12) C1 0.0389(15) 0.0349(15) 0.0358(15) 0.0029(11) 0.0118(12) 0.0011(11) C2 0.0561(19) 0.0381(17) 0.056(2) 0.0005(14) 0.0138(15) -0.0109(15) C3 0.0519(19) 0.0425(17) 0.0431(17) 0.0092(14) 0.0134(14) -0.0049(13) 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_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 S1 C2 . 95.5(2) yes C1 S2 C3 . 94.9(2) yes C1 N1 N1 3_755 111.2(3) yes N1 C1 S2 . 118.9(2) yes N1 C1 S1 . 125.8(2) yes S2 C1 S1 . 115.3(2) yes C3 C2 S1 . 108.1(2) yes C3 C2 H2A . 110.1 no S1 C2 H2A . 110.1 no C3 C2 H2B . 110.1 no S1 C2 H2B . 110.1 no H2A C2 H2B . 108.4 no C2 C3 S2 . 108.8(2) yes C2 C3 H3A . 109.9 no S2 C3 H3A . 109.9 no C2 C3 H3B . 109.9 no S2 C3 H3B . 109.9 no H3A C3 H3B . 108.3 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 C1 . 1.757(3) yes S1 C2 . 1.816(3) yes S2 C1 . 1.749(3) yes S2 C3 . 1.803(3) yes N1 C1 . 1.287(4) yes N1 N1 3_755 1.396(5) yes C2 C3 . 1.506(5) yes C2 H2A . 0.9700 no C2 H2B . 0.9700 no C3 H3A . 0.9700 no C3 H3B . 0.9700 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag N1 N1 C1 S2 3_755 179.1(3) yes N1 N1 C1 S1 3_755 -2.6(5) yes C3 S2 C1 N1 . 164.3(3) yes C3 S2 C1 S1 . -14.2(2) yes C2 S1 C1 N1 . 174.4(3) yes C2 S1 C1 S2 . -7.2(2) yes C1 S1 C2 C3 . 31.4(3) yes S1 C2 C3 S2 . -45.2(3) yes C1 S2 C3 C2 . 36.0(3) yes _cod_database_fobs_code 2204871