Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global #============================================================================== # SUBMISSION DETAILS # ================== _journal_coden_Cambridge 222 _publ_contact_author_name '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 ; Feb 2007 Dear Sirs, This file contains supporting information in CIF format for two crystal structures. Gillian Reid ; _publ_requested_journal 'Dalton Trans.' _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Reversible structural isomerism in rare thioether complexes of cobalt(II) - effects of ligand architecture ; # 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 'Evans, John' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; '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 ; 'Reid, Gillian' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Tsoureas, Nikolaos' ; 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. #============================================================================ # 06nts009 data_06nts009 _database_code_depnum_ccdc_archive 'CCDC 637943' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-01-27 _chemical_name_systematic ; Diiodo(1,2-bis(methylthiomethyl)benzene)cobalt(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H14 Co I2 S2' _chemical_formula_sum 'C10 H14 Co I2 S2' _chemical_formula_weight 511.06 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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/n' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** 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' _cell_length_a 8.3491(15) _cell_length_b 15.467(3) _cell_length_c 11.696(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.917(10) _cell_angle_gamma 90.00 _cell_volume 1509.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3592 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 5.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7671 # 0.6106 _exptl_absorpt_correction_T_max 1.0000 # 0.7714 _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 24660 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.96 _reflns_number_total 3490 _reflns_number_gt 2781 _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^)+(0.0243P)^2^+0.1459P] 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 3490 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0513 _refine_ls_wR_factor_gt 0.0481 _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 Co1 Co 0.21548(4) 0.90825(2) 0.86418(3) 0.02220(9) Uani 1 1 d . . . I1 I 0.00549(2) 0.823319(12) 0.749205(17) 0.03187(7) Uani 1 1 d . . . I2 I 0.20784(2) 0.900714(15) 1.082130(15) 0.03615(7) Uani 1 1 d . . . S1 S 0.48083(8) 0.85910(5) 0.83738(6) 0.02555(16) Uani 1 1 d . . . S2 S 0.19967(7) 1.05129(4) 0.79806(5) 0.02077(14) Uani 1 1 d . . . C1 C 0.4443(4) 0.7467(2) 0.8072(3) 0.0401(8) Uani 1 1 d . . . H1 H 0.3570 0.7414 0.7495 0.060 Uiso 1 1 calc R . . H2 H 0.4145 0.7171 0.8774 0.060 Uiso 1 1 calc R . . H3 H 0.5417 0.7203 0.7781 0.060 Uiso 1 1 calc R . . C2 C 0.5567(3) 0.8971(2) 0.7015(2) 0.0289(7) Uani 1 1 d . . . H4 H 0.6178 0.9511 0.7157 0.035 Uiso 1 1 calc R . . H5 H 0.6323 0.8534 0.6730 0.035 Uiso 1 1 calc R . . C3 C 0.4311(3) 0.91405(18) 0.6094(2) 0.0233(6) Uani 1 1 d . . . C4 C 0.4057(3) 0.8534(2) 0.5235(2) 0.0277(6) Uani 1 1 d . . . H6 H 0.4658 0.8012 0.5249 0.033 Uiso 1 1 calc R . . C5 C 0.2938(3) 0.8678(2) 0.4357(2) 0.0315(7) Uani 1 1 d . . . H7 H 0.2785 0.8258 0.3771 0.038 Uiso 1 1 calc R . . C6 C 0.2047(3) 0.9425(2) 0.4327(2) 0.0292(7) Uani 1 1 d . . . H8 H 0.1268 0.9521 0.3730 0.035 Uiso 1 1 calc R . . C7 C 0.2298(3) 1.00382(19) 0.5181(2) 0.0258(6) Uani 1 1 d . . . H9 H 0.1688 1.0557 0.5157 0.031 Uiso 1 1 calc R . . C8 C 0.3419(3) 0.99123(17) 0.6068(2) 0.0211(6) Uani 1 1 d . . . C9 C 0.3630(3) 1.05978(19) 0.6971(2) 0.0258(6) Uani 1 1 d . . . H10 H 0.3615 1.1177 0.6611 0.031 Uiso 1 1 calc R . . H11 H 0.4675 1.0522 0.7384 0.031 Uiso 1 1 calc R . . C10 C 0.2796(4) 1.1152(2) 0.9160(2) 0.0299(7) Uani 1 1 d . . . H12 H 0.3820 1.0906 0.9434 0.045 Uiso 1 1 calc R . . H13 H 0.2038 1.1148 0.9782 0.045 Uiso 1 1 calc R . . H14 H 0.2962 1.1747 0.8904 0.045 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 Co1 0.02005(18) 0.0244(2) 0.02234(19) 0.00126(15) 0.00274(15) -0.00086(14) I1 0.02102(10) 0.02742(11) 0.04680(13) -0.00138(9) -0.00441(8) -0.00213(7) I2 0.03026(12) 0.05596(15) 0.02263(11) 0.00791(9) 0.00663(8) 0.00196(9) S1 0.0204(3) 0.0346(4) 0.0214(3) -0.0006(3) -0.0021(3) 0.0016(3) S2 0.0201(3) 0.0229(4) 0.0194(3) -0.0023(3) 0.0023(3) -0.0007(3) C1 0.0339(17) 0.0329(18) 0.053(2) 0.0032(16) 0.0017(15) 0.0083(14) C2 0.0178(14) 0.0430(19) 0.0262(15) 0.0026(13) 0.0045(11) 0.0042(12) C3 0.0173(13) 0.0344(16) 0.0185(13) 0.0004(12) 0.0060(11) -0.0008(11) C4 0.0227(14) 0.0325(17) 0.0282(15) -0.0019(13) 0.0072(12) 0.0014(12) C5 0.0281(16) 0.0408(19) 0.0261(15) -0.0103(14) 0.0060(12) -0.0059(13) C6 0.0198(14) 0.047(2) 0.0212(14) 0.0001(13) -0.0006(11) -0.0036(13) C7 0.0199(13) 0.0355(17) 0.0223(14) 0.0036(12) 0.0057(11) -0.0005(12) C8 0.0172(12) 0.0269(15) 0.0195(13) 0.0008(11) 0.0057(10) -0.0034(11) C9 0.0222(14) 0.0316(16) 0.0241(14) -0.0031(12) 0.0077(11) -0.0060(12) C10 0.0360(17) 0.0311(17) 0.0226(15) -0.0070(12) 0.0007(13) -0.0035(13) _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 Co1 S2 2.3460(8) . ? Co1 S1 2.3729(9) . ? Co1 I1 2.5397(5) . ? Co1 I2 2.5546(6) . ? S1 C1 1.798(3) . ? S1 C2 1.828(3) . ? S2 C10 1.806(3) . ? S2 C9 1.838(3) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C2 C3 1.500(4) . ? C2 H4 0.9900 . ? C2 H5 0.9900 . ? C3 C4 1.387(4) . ? C3 C8 1.407(4) . ? C4 C5 1.383(4) . ? C4 H6 0.9500 . ? C5 C6 1.375(4) . ? C5 H7 0.9500 . ? C6 C7 1.387(4) . ? C6 H8 0.9500 . ? C7 C8 1.388(4) . ? C7 H9 0.9500 . ? C8 C9 1.503(4) . ? C9 H10 0.9900 . ? C9 H11 0.9900 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H14 0.9800 . ? 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 S2 Co1 S1 107.52(3) . . ? S2 Co1 I1 106.44(2) . . ? S1 Co1 I1 113.29(3) . . ? S2 Co1 I2 111.65(2) . . ? S1 Co1 I2 99.89(2) . . ? I1 Co1 I2 117.703(17) . . ? C1 S1 C2 101.61(15) . . ? C1 S1 Co1 100.54(10) . . ? C2 S1 Co1 111.35(9) . . ? C10 S2 C9 100.87(13) . . ? C10 S2 Co1 104.40(10) . . ? C9 S2 Co1 104.15(10) . . ? S1 C1 H1 109.5 . . ? S1 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? S1 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C3 C2 S1 115.23(19) . . ? C3 C2 H4 108.5 . . ? S1 C2 H4 108.5 . . ? C3 C2 H5 108.5 . . ? S1 C2 H5 108.5 . . ? H4 C2 H5 107.5 . . ? C4 C3 C8 119.4(2) . . ? C4 C3 C2 119.2(3) . . ? C8 C3 C2 121.4(2) . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H6 119.6 . . ? C3 C4 H6 119.6 . . ? C6 C5 C4 120.4(3) . . ? C6 C5 H7 119.8 . . ? C4 C5 H7 119.8 . . ? C5 C6 C7 119.2(3) . . ? C5 C6 H8 120.4 . . ? C7 C6 H8 120.4 . . ? C6 C7 C8 121.6(3) . . ? C6 C7 H9 119.2 . . ? C8 C7 H9 119.2 . . ? C7 C8 C3 118.6(2) . . ? C7 C8 C9 119.1(2) . . ? C3 C8 C9 122.3(2) . . ? C8 C9 S2 109.23(18) . . ? C8 C9 H10 109.8 . . ? S2 C9 H10 109.8 . . ? C8 C9 H11 109.8 . . ? S2 C9 H11 109.8 . . ? H10 C9 H11 108.3 . . ? S2 C10 H12 109.5 . . ? S2 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? S2 C10 H14 109.5 . . ? H12 C10 H14 109.5 . . ? H13 C10 H14 109.5 . . ? 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 S2 Co1 S1 C1 -146.84(11) . . . . ? I1 Co1 S1 C1 -29.51(12) . . . . ? I2 Co1 S1 C1 96.56(11) . . . . ? S2 Co1 S1 C2 -39.82(11) . . . . ? I1 Co1 S1 C2 77.50(11) . . . . ? I2 Co1 S1 C2 -156.43(11) . . . . ? S1 Co1 S2 C10 -82.46(10) . . . . ? I1 Co1 S2 C10 155.84(10) . . . . ? I2 Co1 S2 C10 26.16(10) . . . . ? S1 Co1 S2 C9 22.94(10) . . . . ? I1 Co1 S2 C9 -98.76(9) . . . . ? I2 Co1 S2 C9 131.55(9) . . . . ? C1 S1 C2 C3 79.1(2) . . . . ? Co1 S1 C2 C3 -27.2(3) . . . . ? S1 C2 C3 C4 -101.4(3) . . . . ? S1 C2 C3 C8 80.4(3) . . . . ? C8 C3 C4 C5 -0.1(4) . . . . ? C2 C3 C4 C5 -178.4(3) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? C4 C5 C6 C7 0.9(4) . . . . ? C5 C6 C7 C8 -0.5(4) . . . . ? C6 C7 C8 C3 -0.2(4) . . . . ? C6 C7 C8 C9 -179.6(2) . . . . ? C4 C3 C8 C7 0.5(4) . . . . ? C2 C3 C8 C7 178.7(2) . . . . ? C4 C3 C8 C9 179.9(2) . . . . ? C2 C3 C8 C9 -1.9(4) . . . . ? C7 C8 C9 S2 78.4(3) . . . . ? C3 C8 C9 S2 -101.0(3) . . . . ? C10 S2 C9 C8 164.2(2) . . . . ? Co1 S2 C9 C8 56.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.470 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.120 #===END OF CIF ============================================================== # 06nts012 data_06nts012 _database_code_depnum_ccdc_archive 'CCDC 637944' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-01-28 _chemical_name_systematic ; Diiodo(tetrakis(methylthiomethyl)methane)cobalt(II) dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H20 Co I2 S4, C H2 Cl2' _chemical_formula_sum 'C10 H22 Cl2 Co I2 S4' _chemical_formula_weight 654.15 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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/n' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** 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' _cell_length_a 8.1358(5) _cell_length_b 10.8094(10) _cell_length_c 23.431(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.816(5) _cell_angle_gamma 90.00 _cell_volume 2036.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4937 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 4.534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7910 # 0.5307 _exptl_absorpt_correction_T_max 1.0000 # 0.8394 _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 37290 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4678 _reflns_number_gt 3935 _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^)+(0.0170P)^2^+1.1849P] 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 4678 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0428 _refine_ls_wR_factor_gt 0.0401 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _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 Co1 Co 0.50799(4) 0.81037(3) 0.364807(13) 0.01249(7) Uani 1 1 d . . . I1 I 0.452645(19) 0.887981(16) 0.251886(7) 0.01751(5) Uani 1 1 d . . . I2 I 0.565767(18) 0.731332(16) 0.479546(7) 0.01639(5) Uani 1 1 d . . . S1 S 0.27437(7) 0.65581(6) 0.34469(3) 0.01431(13) Uani 1 1 d . . . S2 S 0.28608(7) 0.96147(6) 0.38706(3) 0.01472(13) Uani 1 1 d . . . S3 S -0.25307(7) 0.95879(6) 0.38580(3) 0.01401(13) Uani 1 1 d . . . S4 S -0.27609(7) 0.65830(6) 0.34001(3) 0.01389(12) Uani 1 1 d . . . C1 C 0.0083(3) 0.8060(2) 0.36408(10) 0.0132(5) Uani 1 1 d . . . C2 C 0.1267(3) 0.7039(2) 0.39138(10) 0.0149(5) Uani 1 1 d . . . H1 H 0.0603 0.6313 0.4000 0.018 Uiso 1 1 calc R . . H2 H 0.1886 0.7344 0.4284 0.018 Uiso 1 1 calc R . . C3 C 0.3336(3) 0.5088(2) 0.37861(11) 0.0197(6) Uani 1 1 d . . . H3 H 0.3761 0.5219 0.4196 0.030 Uiso 1 1 calc R . . H4 H 0.4205 0.4707 0.3597 0.030 Uiso 1 1 calc R . . H5 H 0.2365 0.4541 0.3749 0.030 Uiso 1 1 calc R . . C4 C 0.1022(3) 0.9096(2) 0.33790(10) 0.0144(5) Uani 1 1 d . . . H6 H 0.0263 0.9806 0.3281 0.017 Uiso 1 1 calc R . . H7 H 0.1369 0.8794 0.3017 0.017 Uiso 1 1 calc R . . C5 C 0.3098(3) 1.1125(2) 0.35581(12) 0.0234(6) Uani 1 1 d . . . H8 H 0.3232 1.1030 0.3152 0.035 Uiso 1 1 calc R . . H9 H 0.4082 1.1535 0.3769 0.035 Uiso 1 1 calc R . . H10 H 0.2109 1.1626 0.3584 0.035 Uiso 1 1 calc R . . C6 C -0.0780(3) 0.8582(2) 0.41256(10) 0.0146(5) Uani 1 1 d . . . H11 H 0.0039 0.9055 0.4397 0.018 Uiso 1 1 calc R . . H12 H -0.1183 0.7887 0.4342 0.018 Uiso 1 1 calc R . . C7 C -0.2649(3) 1.0407(2) 0.45231(11) 0.0210(6) Uani 1 1 d . . . H13 H -0.2665 0.9811 0.4837 0.032 Uiso 1 1 calc R . . H14 H -0.3667 1.0906 0.4479 0.032 Uiso 1 1 calc R . . H15 H -0.1679 1.0950 0.4614 0.032 Uiso 1 1 calc R . . C8 C -0.1176(3) 0.7530(2) 0.31411(10) 0.0150(5) Uani 1 1 d . . . H16 H -0.0575 0.7024 0.2888 0.018 Uiso 1 1 calc R . . H17 H -0.1721 0.8222 0.2908 0.018 Uiso 1 1 calc R . . C9 C -0.3566(3) 0.5823(2) 0.27302(11) 0.0200(6) Uani 1 1 d . . . H18 H -0.3891 0.6447 0.2430 0.030 Uiso 1 1 calc R . . H19 H -0.4538 0.5325 0.2783 0.030 Uiso 1 1 calc R . . H20 H -0.2706 0.5286 0.2613 0.030 Uiso 1 1 calc R . . C10 C -0.2120(3) 0.3835(3) 0.43261(13) 0.0329(7) Uani 1 1 d . . . H21 H -0.2265 0.4743 0.4291 0.039 Uiso 1 1 calc R . . H22 H -0.2789 0.3538 0.4617 0.039 Uiso 1 1 calc R . . Cl1 Cl -0.28468(9) 0.31291(7) 0.36501(3) 0.03789(19) Uani 1 1 d . . . Cl2 Cl 0.00005(9) 0.34912(9) 0.45592(4) 0.0440(2) 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 Co1 0.00853(15) 0.01489(17) 0.01396(17) 0.00024(13) 0.00140(12) -0.00005(13) I1 0.01368(8) 0.02338(10) 0.01541(9) 0.00382(7) 0.00203(6) 0.00125(7) I2 0.01236(8) 0.02204(9) 0.01469(8) 0.00176(7) 0.00183(6) 0.00017(6) S1 0.0104(3) 0.0153(3) 0.0172(3) 0.0007(2) 0.0021(2) 0.0003(2) S2 0.0107(3) 0.0164(3) 0.0168(3) 0.0005(2) 0.0013(2) 0.0002(2) S3 0.0104(3) 0.0157(3) 0.0157(3) -0.0009(2) 0.0011(2) 0.0005(2) S4 0.0102(3) 0.0156(3) 0.0160(3) -0.0005(2) 0.0022(2) -0.0003(2) C1 0.0110(11) 0.0153(13) 0.0131(12) 0.0017(10) 0.0017(9) 0.0012(10) C2 0.0109(11) 0.0182(13) 0.0161(12) 0.0033(10) 0.0037(10) -0.0001(10) C3 0.0165(12) 0.0159(14) 0.0263(14) 0.0030(11) 0.0019(11) 0.0030(11) C4 0.0081(11) 0.0186(14) 0.0163(12) 0.0013(10) 0.0014(9) 0.0010(10) C5 0.0194(13) 0.0176(14) 0.0325(16) 0.0010(12) 0.0022(12) -0.0013(11) C6 0.0095(11) 0.0195(14) 0.0144(12) 0.0018(10) 0.0001(9) 0.0004(10) C7 0.0205(13) 0.0209(15) 0.0206(14) -0.0063(11) -0.0001(11) 0.0006(11) C8 0.0110(11) 0.0201(14) 0.0142(12) 0.0011(10) 0.0025(9) 0.0007(10) C9 0.0175(13) 0.0217(14) 0.0202(14) -0.0068(11) 0.0010(10) 0.0006(11) C10 0.0234(15) 0.0355(18) 0.0407(18) 0.0134(14) 0.0078(13) 0.0047(13) Cl1 0.0344(4) 0.0377(5) 0.0419(5) 0.0118(4) 0.0068(3) 0.0054(4) Cl2 0.0223(4) 0.0572(6) 0.0520(5) 0.0242(4) 0.0039(3) 0.0005(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 Co1 S3 2.5104(7) 1_655 ? Co1 S1 2.5201(7) . ? Co1 S4 2.5375(7) 1_655 ? Co1 S2 2.5471(7) . ? Co1 I1 2.7463(4) . ? Co1 I2 2.7913(4) . ? S1 C3 1.809(3) . ? S1 C2 1.820(2) . ? S2 C5 1.811(3) . ? S2 C4 1.831(2) . ? S3 C7 1.808(2) . ? S3 C6 1.825(2) . ? S3 Co1 2.5104(7) 1_455 ? S4 C9 1.803(3) . ? S4 C8 1.822(2) . ? S4 Co1 2.5375(7) 1_455 ? C1 C6 1.532(3) . ? C1 C4 1.535(3) . ? C1 C2 1.539(3) . ? C1 C8 1.543(3) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 H3 0.9800 . ? C3 H4 0.9800 . ? C3 H5 0.9800 . ? C4 H6 0.9900 . ? C4 H7 0.9900 . ? C5 H8 0.9800 . ? C5 H9 0.9800 . ? C5 H10 0.9800 . ? C6 H11 0.9900 . ? C6 H12 0.9900 . ? C7 H13 0.9800 . ? C7 H14 0.9800 . ? C7 H15 0.9800 . ? C8 H16 0.9900 . ? C8 H17 0.9900 . ? C9 H18 0.9800 . ? C9 H19 0.9800 . ? C9 H20 0.9800 . ? C10 Cl2 1.768(3) . ? C10 Cl1 1.776(3) . ? C10 H21 0.9900 . ? C10 H22 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 S3 Co1 S1 178.19(2) 1_655 . ? S3 Co1 S4 85.20(2) 1_655 1_655 ? S1 Co1 S4 93.24(2) . 1_655 ? S3 Co1 S2 95.85(2) 1_655 . ? S1 Co1 S2 85.73(2) . . ? S4 Co1 S2 178.40(2) 1_655 . ? S3 Co1 I1 90.072(18) 1_655 . ? S1 Co1 I1 90.845(18) . . ? S4 Co1 I1 89.674(17) 1_655 . ? S2 Co1 I1 89.120(17) . . ? S3 Co1 I2 89.761(18) 1_655 . ? S1 Co1 I2 89.317(17) . . ? S4 Co1 I2 90.112(18) 1_655 . ? S2 Co1 I2 91.097(17) . . ? I1 Co1 I2 179.739(13) . . ? C3 S1 C2 98.21(11) . . ? C3 S1 Co1 110.96(9) . . ? C2 S1 Co1 104.30(8) . . ? C5 S2 C4 98.59(12) . . ? C5 S2 Co1 111.86(9) . . ? C4 S2 Co1 102.19(8) . . ? C7 S3 C6 97.92(12) . . ? C7 S3 Co1 109.88(9) . 1_455 ? C6 S3 Co1 103.10(8) . 1_455 ? C9 S4 C8 98.46(12) . . ? C9 S4 Co1 108.81(9) . 1_455 ? C8 S4 Co1 105.21(8) . 1_455 ? C6 C1 C4 109.9(2) . . ? C6 C1 C2 106.55(18) . . ? C4 C1 C2 111.81(18) . . ? C6 C1 C8 111.89(18) . . ? C4 C1 C8 106.29(19) . . ? C2 C1 C8 110.5(2) . . ? C1 C2 S1 112.56(16) . . ? C1 C2 H1 109.1 . . ? S1 C2 H1 109.1 . . ? C1 C2 H2 109.1 . . ? S1 C2 H2 109.1 . . ? H1 C2 H2 107.8 . . ? S1 C3 H3 109.5 . . ? S1 C3 H4 109.5 . . ? H3 C3 H4 109.5 . . ? S1 C3 H5 109.5 . . ? H3 C3 H5 109.5 . . ? H4 C3 H5 109.5 . . ? C1 C4 S2 112.39(16) . . ? C1 C4 H6 109.1 . . ? S2 C4 H6 109.1 . . ? C1 C4 H7 109.1 . . ? S2 C4 H7 109.1 . . ? H6 C4 H7 107.9 . . ? S2 C5 H8 109.5 . . ? S2 C5 H9 109.5 . . ? H8 C5 H9 109.5 . . ? S2 C5 H10 109.5 . . ? H8 C5 H10 109.5 . . ? H9 C5 H10 109.5 . . ? C1 C6 S3 112.77(16) . . ? C1 C6 H11 109.0 . . ? S3 C6 H11 109.0 . . ? C1 C6 H12 109.0 . . ? S3 C6 H12 109.0 . . ? H11 C6 H12 107.8 . . ? S3 C7 H13 109.5 . . ? S3 C7 H14 109.5 . . ? H13 C7 H14 109.5 . . ? S3 C7 H15 109.5 . . ? H13 C7 H15 109.5 . . ? H14 C7 H15 109.5 . . ? C1 C8 S4 112.17(16) . . ? C1 C8 H16 109.2 . . ? S4 C8 H16 109.2 . . ? C1 C8 H17 109.2 . . ? S4 C8 H17 109.2 . . ? H16 C8 H17 107.9 . . ? S4 C9 H18 109.5 . . ? S4 C9 H19 109.5 . . ? H18 C9 H19 109.5 . . ? S4 C9 H20 109.5 . . ? H18 C9 H20 109.5 . . ? H19 C9 H20 109.5 . . ? Cl2 C10 Cl1 111.15(17) . . ? Cl2 C10 H21 109.4 . . ? Cl1 C10 H21 109.4 . . ? Cl2 C10 H22 109.4 . . ? Cl1 C10 H22 109.4 . . ? H21 C10 H22 108.0 . . ? 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 # S3 Co1 S1 C3 16.4(8) 1_655 . . . ? # S3 Co1 S1 C2 121.2(7) 1_655 . . . ? # S4 Co1 S2 C5 -87.0(9) 1_655 . . . ? # S4 Co1 S2 C4 17.6(9) 1_655 . . . ? S4 Co1 S1 C3 46.99(9) 1_655 . . . ? S2 Co1 S1 C3 -134.24(9) . . . . ? I1 Co1 S1 C3 136.71(9) . . . . ? I2 Co1 S1 C3 -43.09(9) . . . . ? S4 Co1 S1 C2 151.78(8) 1_655 . . . ? S2 Co1 S1 C2 -29.45(8) . . . . ? I1 Co1 S1 C2 -118.50(8) . . . . ? I2 Co1 S1 C2 61.71(8) . . . . ? S3 Co1 S2 C5 44.20(10) 1_655 . . . ? S1 Co1 S2 C5 -136.70(10) . . . . ? I1 Co1 S2 C5 -45.79(10) . . . . ? I2 Co1 S2 C5 134.07(10) . . . . ? S3 Co1 S2 C4 148.75(8) 1_655 . . . ? S1 Co1 S2 C4 -32.14(8) . . . . ? I1 Co1 S2 C4 58.77(8) . . . . ? I2 Co1 S2 C4 -121.38(8) . . . . ? C6 C1 C2 S1 -166.68(16) . . . . ? C4 C1 C2 S1 -46.6(2) . . . . ? C8 C1 C2 S1 71.6(2) . . . . ? C3 S1 C2 C1 -161.39(18) . . . . ? Co1 S1 C2 C1 84.43(17) . . . . ? C6 C1 C4 S2 70.8(2) . . . . ? C2 C1 C4 S2 -47.3(2) . . . . ? C8 C1 C4 S2 -167.92(15) . . . . ? C5 S2 C4 C1 -158.76(17) . . . . ? Co1 S2 C4 C1 86.54(16) . . . . ? C4 C1 C6 S3 70.2(2) . . . . ? C2 C1 C6 S3 -168.47(16) . . . . ? C8 C1 C6 S3 -47.7(2) . . . . ? C7 S3 C6 C1 -159.86(18) . . . . ? Co1 S3 C6 C1 87.51(17) 1_455 . . . ? C6 C1 C8 S4 -44.9(2) . . . . ? C4 C1 C8 S4 -164.86(15) . . . . ? C2 C1 C8 S4 73.7(2) . . . . ? C9 S4 C8 C1 -164.90(17) . . . . ? Co1 S4 C8 C1 82.88(16) 1_455 . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.627 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.111 #===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 =============================================================