#------------------------------------------------------------------------------ #$Date: 2010-09-26 12:00:33 +0100 (Sun, 26 Sep 2010) $ #$Revision: 1526 $ #$URL: svn://www.crystallography.net/cod/cif/4/4308322.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_4308322 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 'S Se C5 H8' _chemical_formula_sum 'C5 H8 S Se' _chemical_formula_weight 179.13 _chemical_melting_point 318 _chemical_name_systematic ; 2-thia-6-selenaspiro[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 109.1230(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.8538(5) _cell_length_b 19.4846(18) _cell_length_c 5.8579(5) _cell_measurement_reflns_used 4719 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.20 _cell_measurement_theta_min 3.14 _cell_volume 631.28(10) _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 0.951 _diffrn_measured_fraction_theta_max 0.951 _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 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0179 _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 5332 _diffrn_reflns_theta_full 28.29 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_min 2.09 _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 6.149 _exptl_absorpt_correction_T_max 0.4395 _exptl_absorpt_correction_T_min 0.1455 _exptl_absorpt_correction_type 'multi-scan (SADABS)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_description block _exptl_crystal_F_000 352 _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.426 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.070 _refine_ls_extinction_coef 0.037(2) _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 1.064 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 116 _refine_ls_number_reflns 1486 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.064 _refine_ls_R_factor_all 0.0197 _refine_ls_R_factor_gt 0.0186 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.1178P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.0516 _reflns_number_gt 1417 _reflns_number_total 1486 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic040102g_3.cif _[local]_cod_data_source_block '[SSeC5H8]_(3)' _cod_database_code 4308322 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 Se1 Se 0.3106(7) 0.69704(13) 0.9770(5) 0.0277(5) Uani 0.5953(10) 1 d P . . S1 S 0.292(3) 0.6982(4) 0.9781(17) 0.0223(10) Uani 0.4047(10) 1 d P . . Se2 Se -0.3450(4) 0.57397(17) 0.4040(6) 0.0290(8) Uani 0.4047(10) 1 d P . . S2 S -0.3465(6) 0.5764(3) 0.4061(8) 0.0215(10) Uani 0.5953(10) 1 d P . . C1 C 0.0339(3) 0.65127(8) 1.0213(3) 0.0252(3) Uani 1 1 d . . . C2 C 0.2247(3) 0.62173(9) 0.7510(3) 0.0276(3) Uani 1 1 d . . . H2A H 0.078(4) 0.6189(10) 1.155(3) 0.032(5) Uiso 1 1 d . . . H2B H -0.083(4) 0.6807(10) 1.042(3) 0.029(5) Uiso 1 1 d . . . C3 C -0.0289(2) 0.61823(7) 0.7715(2) 0.0187(3) Uani 1 1 d . . . H3A H 0.318(4) 0.5867(12) 0.821(4) 0.043(6) Uiso 1 1 d . . . H3B H 0.239(4) 0.6299(10) 0.596(4) 0.034(5) Uiso 1 1 d . . . C4 C -0.1557(3) 0.54798(7) 0.7236(3) 0.0266(3) Uani 1 1 d . . . H4A H -0.258(4) 0.5406(10) 0.824(4) 0.039(5) Uiso 1 1 d . . . H4B H -0.055(4) 0.5082(11) 0.734(4) 0.039(5) Uiso 1 1 d . . . C5 C -0.2152(3) 0.65750(7) 0.5645(3) 0.0248(3) Uani 1 1 d . . . H5A H -0.337(4) 0.6825(11) 0.615(4) 0.035(5) Uiso 1 1 d . . . H5B H -0.154(4) 0.6889(10) 0.474(4) 0.034(5) 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 Se1 0.0250(7) 0.0298(7) 0.0246(6) 0.0004(4) 0.0031(3) -0.0086(4) S1 0.0239(17) 0.0198(18) 0.0215(17) -0.0071(12) 0.0052(12) -0.0044(10) Se2 0.0318(12) 0.0208(9) 0.0304(13) -0.0060(6) 0.0050(8) -0.0033(6) S2 0.0135(14) 0.0300(18) 0.0183(16) -0.0034(10) 0.0014(10) -0.0036(9) C1 0.0321(7) 0.0253(7) 0.0197(7) -0.0008(5) 0.0103(6) 0.0013(6) C2 0.0207(7) 0.0361(8) 0.0269(7) -0.0054(6) 0.0089(6) -0.0007(6) C3 0.0192(6) 0.0184(6) 0.0185(6) 0.0005(5) 0.0064(5) 0.0006(5) C4 0.0293(7) 0.0188(7) 0.0301(7) 0.0020(5) 0.0076(6) -0.0011(6) C5 0.0254(7) 0.0209(7) 0.0243(7) 0.0025(5) 0.0031(6) 0.0010(6) 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' Se Se -0.0929 2.2259 '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 Se1 C1 72.59(12) . . y C1 S1 C2 74.0(3) . . y C4 Se2 C5 74.51(13) . . y C5 S2 C4 75.36(17) . . y C3 C1 S1 91.6(3) . . y C3 C1 Se1 90.85(11) . . y S1 C1 Se1 2.2(4) . . y C3 C1 H2A 114.5(11) . . n S1 C1 H2A 114.7(12) . . n Se1 C1 H2A 113.2(12) . . n C3 C1 H2B 115.3(12) . . n S1 C1 H2B 112.4(13) . . n Se1 C1 H2B 114.5(12) . . n H2A C1 H2B 107.9(16) . . n C3 C2 Se1 91.25(15) . . y C3 C2 S1 88.0(4) . . y Se1 C2 S1 3.3(6) . . y C3 C2 H3A 113.2(15) . . n Se1 C2 H3A 106.6(15) . . n S1 C2 H3A 108.5(16) . . n C3 C2 H3B 118.3(12) . . n Se1 C2 H3B 116.2(12) . . n S1 C2 H3B 117.4(13) . . n H3A C2 H3B 109.8(19) . . n C1 C3 C2 96.96(11) . . y C1 C3 C4 119.95(12) . . y C2 C3 C4 116.63(12) . . y C1 C3 C5 115.46(11) . . y C2 C3 C5 111.75(12) . . y C4 C3 C5 97.09(11) . . y C3 C4 Se2 91.90(13) . . y C3 C4 S2 90.72(17) . . y Se2 C4 S2 1.5(3) . . y C3 C4 H4A 112.0(12) . . n Se2 C4 H4A 110.9(13) . . n S2 C4 H4A 110.5(13) . . n C3 C4 H4B 117.2(13) . . n Se2 C4 H4B 114.9(12) . . n S2 C4 H4B 116.3(12) . . n H4A C4 H4B 109.1(17) . . n C3 C5 S2 92.36(16) . . y C3 C5 Se2 91.67(13) . . y S2 C5 Se2 0.8(2) . . y C3 C5 H5A 114.0(12) . . n S2 C5 H5A 110.2(12) . . n Se2 C5 H5A 110.9(12) . . n C3 C5 H5B 117.2(13) . . n S2 C5 H5B 115.9(12) . . n Se2 C5 H5B 115.9(12) . . n H5A C5 H5B 106.8(17) . . 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 Se1 C2 1.929(3) . y Se1 C1 1.940(4) . y S1 C1 1.852(14) . y S1 C2 1.950(7) . y Se2 C4 1.906(3) . y Se2 C5 1.909(4) . y S2 C5 1.865(5) . y S2 C4 1.912(5) . y C1 C3 1.5293(19) . y C1 H2A 0.971(19) . n C1 H2B 0.93(2) . n C2 C3 1.530(2) . y C2 H3A 0.89(2) . n C2 H3B 0.95(2) . n C3 C4 1.5384(19) . y C3 C5 1.5424(19) . y C4 H4A 0.98(2) . n C4 H4B 0.96(2) . n C5 H5A 0.99(2) . n C5 H5B 0.95(2) . n