Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global #============================================================================== # SUBMISSION DETAILS # ================== _journal_coden_Cambridge 222 _publ_contact_author_name 'Professor Gillian Reid' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email gr@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3609' _publ_contact_letter ; November 2007 This file contains crystallographic data in CIF format for two crystal structures. It is being offered as supporting information for a paper to be submitted. Gillian Reid ; _publ_requested_journal 'Dalton Trans.' _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Selenoether macrocyclic chemistry - syntheses and properties of new tridentate and hexadentate Se/O-donor macrocycles ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # Note order: Family_name, first name(s) or initials (or mixture). loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Levason, William' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ? 'Manning, Joanna M.' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ? 'Nirwan, Manisha' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ; Current address: Department of Pure & Applied Chemistry M.D.S University Ajmer, 305009, India ; 'Ratnani, Raju' ; Department of Pure & Applied Chemistry M.D.S University Ajmer, 305009, India ; ? 'Reid, Gillian' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ? 'Smith, Hayley L.' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ? 'Webster, Michael' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ? #============================================================================ # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique (to this file) identifier. #============================================================================ # 06mn003 data_06mn003_[C24H32O2Se4] _database_code_depnum_ccdc_archive 'CCDC 670270' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-06-24 _audit_author_name 'Webster, M.' _chemical_name_systematic ; 6,7,17,18-dibenzo-1,12-dioxa-4,9,15,20-tetraselenacyclodocosa-6,17-diene ; # Name based on systematic names for Refcode PAYSIR (dibenzo-18-crown-6) # and ACUNER (1,12-dithiacyclodocosa-3,9,14,20-tetrayne). _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 O2 Se4' _chemical_formula_sum 'C24 H32 O2 Se4' _chemical_formula_weight 668.34 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** 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' _cell_length_a 9.075(3) _cell_length_b 4.8236(12) _cell_length_c 28.058(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.316(16) _cell_angle_gamma 90.00 _cell_volume 1223.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2625 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 6.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7315 # 0.6446 _exptl_absorpt_correction_T_max 1.0000 # 0.9423 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' # graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11967 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.58 _reflns_number_total 2802 _reflns_number_gt 1992 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0925P)^2^+6.5922P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2802 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1077 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.1955 _refine_ls_wR_factor_gt 0.1738 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 1.05515(8) 0.46521(16) 0.16411(3) 0.0315(3) Uani 1 1 d . . . Se2 Se 0.74873(10) 0.55223(19) 0.05107(3) 0.0376(3) Uani 1 1 d . . . O1 O 1.2402(6) -0.0714(11) 0.07087(19) 0.0340(13) Uani 1 1 d . . . C1 C 0.6502(8) 0.4580(15) 0.1424(3) 0.0275(16) Uani 1 1 d . . . C2 C 0.7577(8) 0.4124(15) 0.1805(3) 0.0271(16) Uani 1 1 d . . . C3 C 0.7483(9) 0.5610(15) 0.2231(3) 0.0330(18) Uani 1 1 d . . . H3 H 0.8198 0.5277 0.2494 0.040 Uiso 1 1 calc R . . C4 C 0.6386(8) 0.7539(16) 0.2279(3) 0.0314(17) Uani 1 1 d . . . H4 H 0.6355 0.8539 0.2569 0.038 Uiso 1 1 calc R . . C5 C 0.5328(9) 0.8001(18) 0.1898(3) 0.0369(19) Uani 1 1 d . . . H5 H 0.4569 0.9332 0.1925 0.044 Uiso 1 1 calc R . . C6 C 0.5380(8) 0.6551(17) 0.1486(3) 0.0319(17) Uani 1 1 d . . . H6 H 0.4637 0.6867 0.1230 0.038 Uiso 1 1 calc R . . C7 C 0.8884(9) 0.2267(17) 0.1772(3) 0.0329(18) Uani 1 1 d . . . H7A H 0.8678 0.0900 0.1511 0.040 Uiso 1 1 calc R . . H7B H 0.9113 0.1251 0.2077 0.040 Uiso 1 1 calc R . . C8 C 1.1854(8) 0.1988(17) 0.1380(3) 0.0322(17) Uani 1 1 d . . . H8A H 1.2840 0.2841 0.1363 0.039 Uiso 1 1 calc R . . H8B H 1.1975 0.0368 0.1596 0.039 Uiso 1 1 calc R . . C9 C 1.1272(9) 0.1018(17) 0.0887(3) 0.0325(17) Uani 1 1 d . . . H9A H 1.0346 -0.0051 0.0903 0.039 Uiso 1 1 calc R . . H9B H 1.1059 0.2626 0.0672 0.039 Uiso 1 1 calc R . . C10 C 1.1912(9) -0.1831(18) 0.0253(3) 0.0328(18) Uani 1 1 d . . . H10A H 1.1718 -0.0318 0.0017 0.039 Uiso 1 1 calc R . . H10B H 1.0983 -0.2887 0.0272 0.039 Uiso 1 1 calc R . . C11 C 1.3112(10) -0.372(2) 0.0101(3) 0.039(2) Uani 1 1 d . . . H11A H 1.3339 -0.5152 0.0350 0.047 Uiso 1 1 calc R . . H11B H 1.4023 -0.2626 0.0073 0.047 Uiso 1 1 calc R . . C12 C 0.6499(9) 0.3099(17) 0.0949(3) 0.0335(18) Uani 1 1 d . . . H12A H 0.5470 0.2715 0.0817 0.040 Uiso 1 1 calc R . . H12B H 0.7033 0.1314 0.0992 0.040 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 Se1 0.0319(5) 0.0276(5) 0.0350(5) -0.0013(3) 0.0038(3) 0.0003(3) Se2 0.0454(5) 0.0415(5) 0.0268(4) -0.0035(3) 0.0078(3) -0.0055(4) O1 0.031(3) 0.041(3) 0.030(3) -0.002(2) -0.001(2) 0.006(2) C1 0.026(4) 0.028(4) 0.029(4) 0.002(3) 0.008(3) -0.007(3) C2 0.034(4) 0.022(4) 0.026(4) 0.005(3) 0.007(3) -0.001(3) C3 0.046(5) 0.025(4) 0.028(4) 0.007(3) 0.001(3) -0.009(3) C4 0.035(4) 0.031(4) 0.028(4) 0.002(3) 0.004(3) 0.002(3) C5 0.031(4) 0.039(5) 0.041(4) 0.003(4) 0.006(4) 0.007(4) C6 0.027(4) 0.031(4) 0.036(4) 0.011(3) -0.004(3) -0.004(3) C7 0.038(4) 0.031(4) 0.031(4) 0.003(3) 0.012(3) -0.002(3) C8 0.029(4) 0.038(5) 0.030(4) 0.001(3) 0.001(3) 0.002(3) C9 0.035(4) 0.036(4) 0.027(4) 0.003(3) 0.004(3) 0.011(3) C10 0.032(4) 0.043(5) 0.024(4) 0.000(3) 0.005(3) 0.008(4) C11 0.041(5) 0.053(5) 0.024(4) -0.007(4) 0.001(3) 0.002(4) C12 0.042(5) 0.029(4) 0.030(4) 0.006(3) 0.000(3) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C8 1.936(8) . ? Se1 C7 1.963(8) . ? Se2 C11 1.957(8) 3_755 ? Se2 C12 1.972(8) . ? O1 C10 1.421(9) . ? O1 C9 1.448(9) . ? C1 C2 1.396(11) . ? C1 C6 1.416(11) . ? C1 C12 1.510(11) . ? C2 C3 1.402(11) . ? C2 C7 1.496(11) . ? C3 C4 1.379(11) . ? C3 H3 0.9500 . ? C4 C5 1.387(11) . ? C4 H4 0.9500 . ? C5 C6 1.355(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.507(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.511(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 Se2 1.957(8) 3_755 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? 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 C8 Se1 C7 101.0(3) . . ? C11 Se2 C12 100.3(4) 3_755 . ? C10 O1 C9 110.9(5) . . ? C2 C1 C6 118.1(7) . . ? C2 C1 C12 123.0(7) . . ? C6 C1 C12 118.9(7) . . ? C1 C2 C3 118.6(7) . . ? C1 C2 C7 123.3(7) . . ? C3 C2 C7 118.0(7) . . ? C4 C3 C2 122.0(7) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 119.1(7) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 119.9(8) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 122.2(7) . . ? C5 C6 H6 118.9 . . ? C1 C6 H6 118.9 . . ? C2 C7 Se1 106.9(5) . . ? C2 C7 H7A 110.3 . . ? Se1 C7 H7A 110.3 . . ? C2 C7 H7B 110.3 . . ? Se1 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? C9 C8 Se1 112.3(5) . . ? C9 C8 H8A 109.1 . . ? Se1 C8 H8A 109.1 . . ? C9 C8 H8B 109.1 . . ? Se1 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? O1 C9 C8 107.2(6) . . ? O1 C9 H9A 110.3 . . ? C8 C9 H9A 110.3 . . ? O1 C9 H9B 110.3 . . ? C8 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? O1 C10 C11 107.9(6) . . ? O1 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? O1 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 C11 Se2 111.4(5) . 3_755 ? C10 C11 H11A 109.3 . . ? Se2 C11 H11A 109.3 3_755 . ? C10 C11 H11B 109.3 . . ? Se2 C11 H11B 109.3 3_755 . ? H11A C11 H11B 108.0 . . ? C1 C12 Se2 107.8(5) . . ? C1 C12 H12A 110.1 . . ? Se2 C12 H12A 110.1 . . ? C1 C12 H12B 110.1 . . ? Se2 C12 H12B 110.1 . . ? H12A C12 H12B 108.5 . . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.7(10) . . . . ? C12 C1 C2 C3 179.8(7) . . . . ? C6 C1 C2 C7 -175.1(7) . . . . ? C12 C1 C2 C7 4.0(11) . . . . ? C1 C2 C3 C4 -1.5(11) . . . . ? C7 C2 C3 C4 174.6(7) . . . . ? C2 C3 C4 C5 0.9(11) . . . . ? C3 C4 C5 C6 0.4(12) . . . . ? C4 C5 C6 C1 -1.1(12) . . . . ? C2 C1 C6 C5 0.5(11) . . . . ? C12 C1 C6 C5 -178.6(7) . . . . ? C1 C2 C7 Se1 97.3(7) . . . . ? C3 C2 C7 Se1 -78.6(7) . . . . ? C8 Se1 C7 C2 -159.7(5) . . . . ? C7 Se1 C8 C9 71.2(6) . . . . ? C10 O1 C9 C8 177.2(7) . . . . ? Se1 C8 C9 O1 173.9(5) . . . . ? C9 O1 C10 C11 -177.2(7) . . . . ? O1 C10 C11 Se2 177.2(5) . . . 3_755 ? C2 C1 C12 Se2 -95.7(7) . . . . ? C6 C1 C12 Se2 83.5(7) . . . . ? C11 Se2 C12 C1 -165.5(5) 3_755 . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.250 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.172 #===END OF CIF ============================================================== # 07sdr015 data_07sdr015_[C12H16OSe2] _database_code_depnum_ccdc_archive 'CCDC 670271' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-10-10 _audit_author_name 'Webster, M.' _chemical_name_systematic ; 9,10-benzo-1,7-diselena-4-oxa-cycloundeca-9-ene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H16 O Se2' _chemical_formula_sum 'C12 H16 O Se2' _chemical_formula_weight 334.17 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9226(15) _cell_length_b 7.9778(15) _cell_length_c 10.1088(15) _cell_angle_alpha 108.104(10) _cell_angle_beta 92.404(10) _cell_angle_gamma 91.037(10) _cell_volume 606.43(19) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2736 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 6.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6414 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13054 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.55 _reflns_number_total 2783 _reflns_number_gt 2406 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+1.1144P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2783 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.29853(4) 0.20941(4) 0.82231(3) 0.01643(10) Uani 1 1 d . . . Se2 Se 0.68227(4) -0.27965(4) 0.69455(3) 0.01768(10) Uani 1 1 d . . . O1 O 0.2987(3) -0.2105(3) 0.7895(2) 0.0178(4) Uani 1 1 d . . . C1 C 0.5179(4) 0.1463(4) 0.8922(3) 0.0174(6) Uani 1 1 d . . . H1A H 0.5385 0.2153 0.9917 0.021 Uiso 1 1 calc R . . H1B H 0.5148 0.0195 0.8846 0.021 Uiso 1 1 calc R . . C2 C 0.1499(4) 0.0548(4) 0.8875(3) 0.0194(6) Uani 1 1 d . . . H2A H 0.1930 0.0545 0.9808 0.023 Uiso 1 1 calc R . . H2B H 0.0354 0.1036 0.8974 0.023 Uiso 1 1 calc R . . C3 C 0.1370(4) -0.1341(4) 0.7907(3) 0.0180(6) Uani 1 1 d . . . H3A H 0.0522 -0.2029 0.8235 0.022 Uiso 1 1 calc R . . H3B H 0.1007 -0.1358 0.6953 0.022 Uiso 1 1 calc R . . C4 C 0.3137(4) -0.3663(4) 0.6761(3) 0.0192(6) Uani 1 1 d . . . H4A H 0.2987 -0.3396 0.5871 0.023 Uiso 1 1 calc R . . H4B H 0.2252 -0.4545 0.6781 0.023 Uiso 1 1 calc R . . C5 C 0.4866(4) -0.4394(4) 0.6867(3) 0.0192(6) Uani 1 1 d . . . H5A H 0.4965 -0.5463 0.6055 0.023 Uiso 1 1 calc R . . H5B H 0.4936 -0.4769 0.7714 0.023 Uiso 1 1 calc R . . C6 C 0.5885(4) -0.1020(4) 0.6142(3) 0.0162(6) Uani 1 1 d . . . H6A H 0.5956 -0.1430 0.5116 0.019 Uiso 1 1 calc R . . H6B H 0.4683 -0.0837 0.6361 0.019 Uiso 1 1 calc R . . C7 C 0.6895(4) 0.0670(4) 0.6760(3) 0.0140(6) Uani 1 1 d . . . C8 C 0.8196(4) 0.1108(4) 0.6016(3) 0.0179(6) Uani 1 1 d . . . H8 H 0.8416 0.0327 0.5122 0.021 Uiso 1 1 calc R . . C9 C 0.9173(4) 0.2657(4) 0.6556(4) 0.0216(7) Uani 1 1 d . . . H9 H 1.0036 0.2938 0.6027 0.026 Uiso 1 1 calc R . . C10 C 0.8876(4) 0.3793(4) 0.7873(4) 0.0221(7) Uani 1 1 d . . . H10 H 0.9546 0.4847 0.8256 0.027 Uiso 1 1 calc R . . C11 C 0.7593(4) 0.3375(4) 0.8628(3) 0.0193(6) Uani 1 1 d . . . H11 H 0.7399 0.4154 0.9529 0.023 Uiso 1 1 calc R . . C12 C 0.6585(4) 0.1840(4) 0.8092(3) 0.0146(6) Uani 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 0.01507(16) 0.01507(17) 0.01938(17) 0.00568(12) 0.00067(11) 0.00151(11) Se2 0.01526(16) 0.01355(17) 0.02369(18) 0.00572(13) -0.00422(12) -0.00009(12) O1 0.0177(11) 0.0159(11) 0.0182(11) 0.0030(9) -0.0005(8) 0.0018(9) C1 0.0167(14) 0.0210(16) 0.0125(14) 0.0029(12) -0.0030(11) 0.0017(12) C2 0.0172(15) 0.0220(16) 0.0185(15) 0.0053(13) 0.0049(12) 0.0028(12) C3 0.0124(14) 0.0197(16) 0.0222(16) 0.0075(13) -0.0004(12) -0.0022(12) C4 0.0181(15) 0.0146(15) 0.0225(16) 0.0028(12) -0.0021(12) -0.0048(12) C5 0.0210(15) 0.0115(14) 0.0239(16) 0.0038(12) 0.0002(12) -0.0005(12) C6 0.0157(14) 0.0144(15) 0.0192(15) 0.0064(12) -0.0021(11) 0.0020(11) C7 0.0133(13) 0.0126(14) 0.0170(15) 0.0066(11) -0.0045(11) 0.0006(11) C8 0.0152(14) 0.0203(16) 0.0192(15) 0.0080(12) -0.0018(12) 0.0010(12) C9 0.0149(15) 0.0226(17) 0.0319(18) 0.0159(14) -0.0029(13) -0.0020(12) C10 0.0165(15) 0.0144(15) 0.0366(19) 0.0109(14) -0.0077(13) -0.0023(12) C11 0.0193(15) 0.0128(15) 0.0238(16) 0.0036(12) -0.0056(12) 0.0007(12) C12 0.0154(14) 0.0120(14) 0.0156(14) 0.0036(11) -0.0039(11) 0.0020(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 1.965(3) . ? Se1 C1 1.981(3) . ? Se2 C5 1.972(3) . ? Se2 C6 1.981(3) . ? O1 C4 1.416(4) . ? O1 C3 1.427(4) . ? C1 C12 1.503(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.520(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.511(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.498(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.401(4) . ? C7 C12 1.414(4) . ? C8 C9 1.391(4) . ? C8 H8 0.9500 . ? C9 C10 1.391(5) . ? C9 H9 0.9500 . ? C10 C11 1.392(5) . ? C10 H10 0.9500 . ? C11 C12 1.396(4) . ? C11 H11 0.9500 . ? 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 98.42(13) . . ? C5 Se2 C6 103.47(13) . . ? C4 O1 C3 113.1(2) . . ? C12 C1 Se1 110.1(2) . . ? C12 C1 H1A 109.6 . . ? Se1 C1 H1A 109.6 . . ? C12 C1 H1B 109.6 . . ? Se1 C1 H1B 109.6 . . ? H1A C1 H1B 108.2 . . ? C3 C2 Se1 113.4(2) . . ? C3 C2 H2A 108.9 . . ? Se1 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? Se1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O1 C3 C2 108.6(2) . . ? O1 C3 H3A 110.0 . . ? C2 C3 H3A 110.0 . . ? O1 C3 H3B 110.0 . . ? C2 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? O1 C4 C5 109.0(2) . . ? O1 C4 H4A 109.9 . . ? C5 C4 H4A 109.9 . . ? O1 C4 H4B 109.9 . . ? C5 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C4 C5 Se2 116.6(2) . . ? C4 C5 H5A 108.1 . . ? Se2 C5 H5A 108.1 . . ? C4 C5 H5B 108.1 . . ? Se2 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C7 C6 Se2 108.02(19) . . ? C7 C6 H6A 110.1 . . ? Se2 C6 H6A 110.1 . . ? C7 C6 H6B 110.1 . . ? Se2 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C8 C7 C12 118.7(3) . . ? C8 C7 C6 119.7(3) . . ? C12 C7 C6 121.6(3) . . ? C9 C8 C7 121.6(3) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 119.6(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 121.5(3) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C7 119.1(3) . . ? C11 C12 C1 119.9(3) . . ? C7 C12 C1 121.0(3) . . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Se1 C1 C12 156.3(2) . . . . ? C1 Se1 C2 C3 -82.4(2) . . . . ? C4 O1 C3 C2 -163.7(3) . . . . ? Se1 C2 C3 O1 65.2(3) . . . . ? C3 O1 C4 C5 -178.3(2) . . . . ? O1 C4 C5 Se2 -56.4(3) . . . . ? C6 Se2 C5 C4 -21.0(3) . . . . ? C5 Se2 C6 C7 152.1(2) . . . . ? Se2 C6 C7 C8 98.1(3) . . . . ? Se2 C6 C7 C12 -81.2(3) . . . . ? C12 C7 C8 C9 -0.2(4) . . . . ? C6 C7 C8 C9 -179.5(3) . . . . ? C7 C8 C9 C10 1.0(5) . . . . ? C8 C9 C10 C11 -0.8(5) . . . . ? C9 C10 C11 C12 -0.2(5) . . . . ? C10 C11 C12 C7 1.0(4) . . . . ? C10 C11 C12 C1 -178.2(3) . . . . ? C8 C7 C12 C11 -0.8(4) . . . . ? C6 C7 C12 C11 178.5(3) . . . . ? C8 C7 C12 C1 178.5(3) . . . . ? C6 C7 C12 C1 -2.3(4) . . . . ? Se1 C1 C12 C11 100.3(3) . . . . ? Se1 C1 C12 C7 -78.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.488 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.121 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================