#------------------------------------------------------------------------------ #$Date: 2014-07-11 23:16:09 +0100 (Fri, 11 Jul 2014) $ #$Revision: 120081 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/83/4308321.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_4308321 loop_ _publ_author_name 'Marina A. Petrukhina' 'Colin Henck' 'Bo Li' 'Eric Block' 'Jin Jin' 'Shao-Zhong Zhang' 'Rodolphe Clerac' _publ_section_title ; Spirocyclic Sulfur and Selenium Ligands as Molecular Rigid Rods in Coordination of Transition Metal Centers ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 77 _journal_page_last 84 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'S2 C5 H8' _chemical_formula_sum 'C5 H8 S2' _chemical_formula_weight 132.23 _chemical_melting_point 304 _chemical_name_systematic ; 2,6-dithiaspiro[3.3]heptane ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 109.7090(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.8013(4) _cell_length_b 19.2532(12) _cell_length_c 5.8183(4) _cell_measurement_reflns_used 4441 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.20 _cell_measurement_theta_min 3.73 _cell_volume 611.80(7) _computing_cell_refinement 'SMART, SAINT' _computing_data_collection SMART _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXP-93 (Sheldrick, 1993)' _computing_publication_material 'SHELXCIF-93 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measurement_device_type 'Brucker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _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 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0124 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 5251 _diffrn_reflns_theta_full 28.16 _diffrn_reflns_theta_max 28.16 _diffrn_reflns_theta_min 2.12 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_number 'none (area dectector data)' _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_T_max 0.9641 _exptl_absorpt_correction_T_min 0.8373 _exptl_absorpt_correction_type 'multi-scan (SADABS)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_description block _exptl_crystal_F_000 280 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.269 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.084 _refine_ls_extinction_coef noref _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 96 _refine_ls_number_reflns 1437 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0253 _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^)+(0.0408P)^2^+0.1677P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.0691 _reflns_number_gt 1355 _reflns_number_total 1437 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic040102g_2.cif _[local]_cod_data_source_block '[S2C5H8]_(1)' _cod_database_code 4308321 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, 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 0.34421(5) 0.424708(16) 0.59029(6) 0.02826(12) Uani 1 1 d . . . S2 S -0.29987(6) 0.303784(17) 0.02130(6) 0.03027(12) Uani 1 1 d . . . C1 C 0.1550(2) 0.45228(6) 0.2820(2) 0.0263(3) Uani 1 1 d . . . H1A H 0.057(3) 0.4915(9) 0.281(3) 0.036(4) Uiso 1 1 d . . . H1B H 0.254(3) 0.4615(9) 0.182(3) 0.041(5) Uiso 1 1 d . . . C2 C 0.2202(2) 0.34250(6) 0.4420(2) 0.0245(2) Uani 1 1 d . . . H2A H 0.158(3) 0.3110(9) 0.539(3) 0.039(5) Uiso 1 1 d . . . H2B H 0.338(3) 0.3182(9) 0.398(3) 0.037(4) Uiso 1 1 d . . . C3 C 0.0291(2) 0.38105(6) 0.2300(2) 0.0196(2) Uani 1 1 d . . . C4 C -0.0361(2) 0.34719(7) -0.0222(2) 0.0253(2) Uani 1 1 d . . . H4A H -0.091(3) 0.3803(8) -0.152(3) 0.030(4) Uiso 1 1 d . . . H4B H 0.083(3) 0.3174(8) -0.046(3) 0.029(4) Uiso 1 1 d . . . C5 C -0.2302(2) 0.37538(7) 0.2431(2) 0.0279(3) Uani 1 1 d . . . H5A H -0.328(3) 0.4151(10) 0.168(3) 0.039(5) Uiso 1 1 d . . . H5B H -0.242(3) 0.3639(8) 0.400(3) 0.036(4) Uiso 1 1 d . . . 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 0.02446(18) 0.02814(19) 0.02679(19) -0.00519(11) 0.00155(13) -0.00329(11) S2 0.02819(19) 0.03173(19) 0.02602(18) -0.00213(11) 0.00274(13) -0.00958(12) C1 0.0251(6) 0.0212(6) 0.0299(6) 0.0003(5) 0.0056(5) -0.0014(4) C2 0.0227(6) 0.0223(5) 0.0242(6) 0.0001(4) 0.0025(5) -0.0004(4) C3 0.0182(5) 0.0206(5) 0.0197(5) -0.0004(4) 0.0061(4) 0.0002(4) C4 0.0295(6) 0.0266(6) 0.0205(5) -0.0013(5) 0.0094(5) -0.0020(5) C5 0.0193(5) 0.0367(7) 0.0280(6) -0.0062(5) 0.0083(5) -0.0018(5) 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' 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 C2 S1 C1 77.24(6) . . y C4 S2 C5 76.05(6) . . y C3 C1 S1 91.29(7) . . y C3 C1 H1A 117.8(10) . . n S1 C1 H1A 113.3(11) . . n C3 C1 H1B 112.8(11) . . n S1 C1 H1B 111.2(11) . . n H1A C1 H1B 109.4(14) . . n C3 C2 S1 91.33(7) . . y C3 C2 H2A 117.1(11) . . n S1 C2 H2A 115.2(10) . . n C3 C2 H2B 114.8(11) . . n S1 C2 H2B 110.8(11) . . n H2A C2 H2B 107.1(14) . . n C4 C3 C1 121.09(10) . . y C4 C3 C5 95.05(9) . . y C1 C3 C5 117.56(10) . . y C4 C3 C2 116.08(10) . . y C1 C3 C2 96.09(9) . . y C5 C3 C2 112.22(10) . . y C3 C4 S2 90.55(7) . . y C3 C4 H4A 112.5(9) . . n S2 C4 H4A 109.8(10) . . n C3 C4 H4B 116.3(10) . . n S2 C4 H4B 115.3(10) . . n H4A C4 H4B 110.8(13) . . n C3 C5 S2 90.33(7) . . y C3 C5 H5A 111.0(11) . . n S2 C5 H5A 108.7(11) . . n C3 C5 H5B 116.6(10) . . n S2 C5 H5B 115.1(10) . . n H5A C5 H5B 113.0(15) . . n 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 1.8299(12) . y S1 C1 1.8373(13) . y S2 C4 1.8346(13) . y S2 C5 1.8377(13) . y C1 C3 1.5353(16) . y C1 H1A 0.945(17) . n C1 H1B 0.960(18) . n C2 C3 1.5426(16) . y C2 H2A 0.978(17) . n C2 H2B 0.933(18) . n C3 C4 1.5318(16) . y C3 C5 1.5351(16) . y C4 H4A 0.959(16) . n C4 H4B 0.941(16) . n C5 H5A 0.963(18) . n C5 H5B 0.962(17) . n _journal_paper_doi 10.1021/ic040102g