#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2204812.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_2204812 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Tiina Maaninen' 'Jari Konu' 'Risto S. Laitinen' _publ_section_title ; A low-temperature redetermination of the monoclinic \b-form of cyclooctaselenium ; _journal_issue 12 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first o2235 _journal_page_last o2237 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac Se8 _chemical_formula_moiety Se8 _chemical_formula_structural Se8 _chemical_formula_sum Se8 _chemical_formula_weight 631.68 _chemical_name_systematic ; beta-monoclinic cyclooctaselenium ; _symmetry_cell_setting monoclinic _atom_sites_solution_hydrogens none _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 92.95(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.2004(18) _cell_length_b 8.0000(16) _cell_length_c 12.735(3) _cell_measurement_reflns_used 9298 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.00 _cell_measurement_theta_min 2.22 _cell_volume 936.1(3) _computing_cell_refinement 'DENZO--SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_data_reduction DENZO--SMN _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'WINGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _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 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 9298 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.22 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 31.143 _exptl_absorpt_correction_T_max 0.2105 _exptl_absorpt_correction_T_min 0.0617 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(SHELXTL; Bruker, 2001)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 4.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1088 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.133 _refine_diff_density_min -1.228 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 1821 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.091 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0400 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0413P)^2^+5.4999P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.0954 _reflns_number_gt 1463 _reflns_number_total 1821 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wm6031.cif 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_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_occupancy _atom_site_type_symbol Se1 0.06355(10) 0.68641(11) 0.91290(7) 0.0288(2) Uani d 1 Se Se2 0.25586(11) 0.77285(11) 1.02241(8) 0.0304(3) Uani d 1 Se Se3 0.25827(11) 0.60084(11) 1.16858(7) 0.0279(2) Uani d 1 Se Se4 0.44886(10) 0.41857(11) 1.14620(7) 0.0256(2) Uani d 1 Se Se5 0.34045(11) 0.17089(11) 1.09083(7) 0.0270(2) Uani d 1 Se Se6 0.35943(10) 0.16250(11) 0.90960(7) 0.0240(2) Uani d 1 Se Se7 0.13558(10) 0.24704(12) 0.84010(7) 0.0297(3) Uani d 1 Se Se8 0.16495(11) 0.52018(13) 0.78818(7) 0.0329(3) Uani d 1 Se 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 Se1 0.0278(5) 0.0309(5) 0.0278(5) 0.0072(4) 0.0030(4) 0.0012(4) Se2 0.0354(6) 0.0211(5) 0.0350(6) -0.0020(4) 0.0058(4) 0.0020(4) Se3 0.0337(6) 0.0245(5) 0.0261(5) 0.0009(4) 0.0075(4) -0.0018(4) Se4 0.0241(5) 0.0279(5) 0.0246(5) -0.0011(4) 0.0005(4) -0.0008(4) Se5 0.0358(6) 0.0223(5) 0.0236(5) -0.0006(4) 0.0068(4) 0.0026(3) Se6 0.0281(5) 0.0208(5) 0.0235(5) 0.0008(4) 0.0057(4) 0.0002(3) Se7 0.0246(5) 0.0364(6) 0.0283(5) -0.0029(4) 0.0022(4) -0.0082(4) Se8 0.0342(6) 0.0398(6) 0.0251(5) 0.0104(4) 0.0040(4) 0.0043(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Se1 Se2 2.3021(15) Se1 Se8 2.3052(14) Se2 Se3 2.3141(14) Se3 Se4 2.3095(14) Se4 Se5 2.3121(13) Se5 Se6 2.3244(13) Se6 Se7 2.3010(15) Se7 Se8 2.3029(15) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Se2 Se1 Se8 105.37(5) no Se1 Se2 Se3 106.50(5) no Se4 Se3 Se2 104.60(5) no Se3 Se4 Se5 105.09(5) no Se4 Se5 Se6 105.92(5) no Se7 Se6 Se5 105.19(5) no Se6 Se7 Se8 105.87(5) no Se7 Se8 Se1 106.97(5) 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 _geom_torsion_publ_flag Se8 Se1 Se2 Se3 -99.24(6) no Se1 Se2 Se3 Se4 104.27(6) no Se2 Se3 Se4 Se5 -103.15(6) no Se3 Se4 Se5 Se6 100.28(6) no Se4 Se5 Se6 Se7 -99.75(6) no Se5 Se6 Se7 Se8 102.57(5) no Se6 Se7 Se8 Se1 -103.24(6) no Se2 Se1 Se8 Se7 98.21(6) no _cod_database_code 2204812