Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_cu4m data_global _database_code_CSD 177918 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Persson, Ingmar' 'Persson, Per' 'Sandstrom, Magnus' 'Ullstrom, Ann-Sofi' _publ_contact_author_name 'Prof Ingmar Persson' _publ_contact_author_address ; Department of Chemistry Swedish University of Argricultural Sciences P O Box 7015 Uppsala SE-750 07 SWEDEN ; _publ_contact_author_email 'INGMAR.PERSSON@KEMI.SLU.SE' _publ_section_title ; Structure of Jahn-Teller Distorted Solvated Copper (II) Ions in Solution, and in Solids with Apparently Regular Octahedral Coordination Geometry ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H48 Cl2 Cu O16 S8' _chemical_formula_weight 887.46 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' 'S' 'S' 0.1246 0.1234 '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' 'Cu' 'Cu' 0.3201 1.2651 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.772(4) _cell_length_b 10.551(4) _cell_length_c 11.563(4) _cell_angle_alpha 64.237(6) _cell_angle_beta 71.779(6) _cell_angle_gamma 87.448(7) _cell_volume 1014.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6389 _cell_measurement_theta_min 28.72 _cell_measurement_theta_max 2.16 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 463 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type 'Bruker Sadabs' _exptl_absorpt_correction_T_min 0.4278 _exptl_absorpt_correction_T_max 0.6288 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD 1k' _diffrn_measurement_method 'Bruker Smart' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6389 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.1701 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.72 _reflns_number_total 4625 _reflns_number_gt 1707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Saintplus' _computing_data_reduction 'Bruker Saintplus' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker Shelxtl-nt' _computing_publication_material 'Bruker Shelxtl-nt' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0170(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4625 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 0.665 _refine_ls_restrained_S_all 0.665 _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 Cu1 Cu 0.5000 0.0000 0.0000 0.0484(3) Uani 1 2 d S . . S2 S 0.29147(15) -0.00595(16) 0.27569(15) 0.0816(5) Uani 1 1 d . . . S3 S 0.65201(14) 0.00715(13) 0.19356(12) 0.0619(4) Uani 1 1 d . . . Cl1 Cl 0.28421(18) 0.27583(16) 0.43967(15) 0.0813(4) Uani 1 1 d . . . S1 S 0.52016(14) -0.31919(13) 0.14091(14) 0.0674(4) Uani 1 1 d . . . S5 S 0.08224(19) -0.40605(16) 0.11572(17) 0.0962(5) Uani 1 1 d . . . O1 O 0.6036(3) -0.1718(3) 0.0558(3) 0.0599(8) Uani 1 1 d . . . O2 O 0.3330(4) -0.0941(3) 0.1991(3) 0.0759(10) Uani 1 1 d . . . O3 O 0.6228(3) 0.0989(3) 0.0619(3) 0.0655(9) Uani 1 1 d . . . O8 O -0.0155(5) -0.3155(4) 0.0445(4) 0.1124(14) Uani 1 1 d . . . O7 O 0.3219(5) 0.3431(5) 0.3003(4) 0.1312(17) Uani 1 1 d . . . C9 C 0.8319(5) -0.0356(5) 0.1462(5) 0.0794(15) Uani 1 1 d . . . H9A H 0.8358 -0.1006 0.1078 0.119 Uiso 1 1 calc R . . H9B H 0.8624 -0.0784 0.2249 0.119 Uiso 1 1 calc R . . H9C H 0.8948 0.0491 0.0802 0.119 Uiso 1 1 calc R . . C8 C 0.0932(7) -0.3482(6) 0.2341(6) 0.1002(19) Uani 1 1 d . . . H8A H 0.1366 -0.2519 0.1871 0.150 Uiso 1 1 calc R . . H8B H 0.1512 -0.4071 0.2857 0.150 Uiso 1 1 calc R . . H8C H -0.0024 -0.3540 0.2943 0.150 Uiso 1 1 calc R . . C7 C 0.5675(8) -0.3860(5) 0.2882(5) 0.107(2) Uani 1 1 d . . . H7A H 0.6693 -0.3959 0.2660 0.160 Uiso 1 1 calc R . . H7B H 0.5137 -0.4768 0.3509 0.160 Uiso 1 1 calc R . . H7C H 0.5454 -0.3222 0.3290 0.160 Uiso 1 1 calc R . . C6 C 0.6823(7) 0.1297(6) 0.2520(6) 0.0940(18) Uani 1 1 d . . . H6A H 0.7564 0.2032 0.1815 0.141 Uiso 1 1 calc R . . H6B H 0.7127 0.0819 0.3303 0.141 Uiso 1 1 calc R . . H6C H 0.5943 0.1704 0.2757 0.141 Uiso 1 1 calc R . . O6 O 0.4042(7) 0.2241(6) 0.4769(5) 0.187(3) Uani 1 1 d . . . C5 C 0.1260(6) 0.0574(6) 0.2574(6) 0.1016(19) Uani 1 1 d . . . H5A H 0.1379 0.1118 0.1627 0.152 Uiso 1 1 calc R . . H5B H 0.0964 0.1161 0.3033 0.152 Uiso 1 1 calc R . . H5C H 0.0533 -0.0211 0.2962 0.152 Uiso 1 1 calc R . . C4 C 0.6258(7) -0.4176(6) 0.0599(6) 0.116(2) Uani 1 1 d . . . H4A H 0.6197 -0.3842 -0.0298 0.174 Uiso 1 1 calc R . . H4B H 0.5898 -0.5160 0.1118 0.174 Uiso 1 1 calc R . . H4C H 0.7250 -0.4056 0.0539 0.174 Uiso 1 1 calc R . . O5 O 0.2448(7) 0.3738(7) 0.4884(6) 0.191(3) Uani 1 1 d . . . O4 O 0.1759(7) 0.1680(6) 0.4950(6) 0.204(3) Uani 1 1 d . . . C3 C -0.0181(8) -0.5692(6) 0.2272(7) 0.143(3) Uani 1 1 d . . . H3A H -0.1040 -0.5566 0.2884 0.214 Uiso 1 1 calc R . . H3B H 0.0390 -0.6307 0.2782 0.214 Uiso 1 1 calc R . . H3C H -0.0448 -0.6103 0.1768 0.214 Uiso 1 1 calc R . . C2 C 0.2264(8) -0.1323(7) 0.4454(6) 0.129(2) Uani 1 1 d . . . H2A H 0.1485 -0.1941 0.4575 0.194 Uiso 1 1 calc R . . H2B H 0.1919 -0.0857 0.5025 0.194 Uiso 1 1 calc R . . H2C H 0.3031 -0.1867 0.4693 0.194 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 Cu1 0.0409(5) 0.0555(5) 0.0456(5) -0.0195(4) -0.0145(4) 0.0079(4) S2 0.0562(10) 0.1111(11) 0.0895(11) -0.0594(10) -0.0164(8) 0.0033(8) S3 0.0497(8) 0.0759(8) 0.0497(7) -0.0189(6) -0.0156(6) 0.0055(7) Cl1 0.0792(12) 0.0825(10) 0.0643(10) -0.0207(8) -0.0174(8) 0.0066(9) S1 0.0536(9) 0.0633(8) 0.0765(9) -0.0225(7) -0.0222(7) 0.0041(7) S5 0.0952(13) 0.0850(11) 0.1022(13) -0.0367(9) -0.0316(10) 0.0124(10) O1 0.042(2) 0.0648(19) 0.068(2) -0.0231(16) -0.0221(16) 0.0084(16) O2 0.077(3) 0.074(2) 0.080(2) -0.0400(19) -0.020(2) 0.0043(19) O3 0.065(2) 0.070(2) 0.0536(19) -0.0192(16) -0.0219(17) 0.0089(17) O8 0.130(4) 0.079(2) 0.120(3) -0.017(2) -0.072(3) 0.017(3) O7 0.146(5) 0.144(4) 0.065(3) -0.017(3) -0.027(3) 0.006(3) C9 0.057(4) 0.082(3) 0.094(4) -0.032(3) -0.029(3) 0.015(3) C8 0.098(5) 0.102(4) 0.119(5) -0.058(4) -0.048(4) 0.025(4) C7 0.147(6) 0.075(4) 0.086(4) -0.014(3) -0.054(4) -0.004(4) C6 0.101(5) 0.111(4) 0.087(4) -0.056(4) -0.037(4) 0.024(4) O6 0.147(5) 0.234(6) 0.154(5) -0.051(4) -0.075(4) 0.094(5) C5 0.061(4) 0.137(5) 0.109(5) -0.059(4) -0.027(4) 0.027(4) C4 0.131(6) 0.075(4) 0.134(6) -0.057(4) -0.017(5) 0.008(4) O5 0.211(7) 0.202(5) 0.185(6) -0.127(5) -0.043(5) 0.061(5) O4 0.195(7) 0.204(5) 0.145(5) -0.033(4) -0.017(4) -0.116(5) C3 0.141(7) 0.091(4) 0.177(7) -0.012(5) -0.096(6) -0.008(4) C2 0.140(7) 0.170(6) 0.076(4) -0.051(4) -0.041(5) 0.025(5) _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 Cu1 O1 1.989(3) 2_655 ? Cu1 O1 1.989(3) . ? Cu1 O3 2.083(3) . ? Cu1 O3 2.083(3) 2_655 ? Cu1 O2 2.181(3) . ? Cu1 O2 2.181(3) 2_655 ? S2 O2 1.507(3) . ? S2 C2 1.747(6) . ? S2 C5 1.761(5) . ? S3 O3 1.518(3) . ? S3 C6 1.770(5) . ? S3 C9 1.770(5) . ? Cl1 O5 1.367(5) . ? Cl1 O4 1.370(5) . ? Cl1 O7 1.376(4) . ? Cl1 O6 1.383(5) . ? S1 O1 1.527(3) . ? S1 C7 1.741(5) . ? S1 C4 1.779(6) . ? S5 O8 1.493(4) . ? S5 C3 1.737(6) . ? S5 C8 1.755(5) . ? 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 O1 Cu1 O1 180.0(2) 2_655 . ? O1 Cu1 O3 89.05(12) 2_655 . ? O1 Cu1 O3 90.95(12) . . ? O1 Cu1 O3 90.95(12) 2_655 2_655 ? O1 Cu1 O3 89.05(12) . 2_655 ? O3 Cu1 O3 180.00(17) . 2_655 ? O1 Cu1 O2 90.34(12) 2_655 . ? O1 Cu1 O2 89.66(12) . . ? O3 Cu1 O2 93.06(12) . . ? O3 Cu1 O2 86.94(12) 2_655 . ? O1 Cu1 O2 89.66(12) 2_655 2_655 ? O1 Cu1 O2 90.34(12) . 2_655 ? O3 Cu1 O2 86.94(12) . 2_655 ? O3 Cu1 O2 93.06(12) 2_655 2_655 ? O2 Cu1 O2 180.0 . 2_655 ? O2 S2 C2 103.4(3) . . ? O2 S2 C5 106.7(2) . . ? C2 S2 C5 98.6(3) . . ? O3 S3 C6 103.7(2) . . ? O3 S3 C9 106.0(2) . . ? C6 S3 C9 98.4(3) . . ? O5 Cl1 O4 111.7(4) . . ? O5 Cl1 O7 108.7(3) . . ? O4 Cl1 O7 111.1(3) . . ? O5 Cl1 O6 105.2(4) . . ? O4 Cl1 O6 110.1(4) . . ? O7 Cl1 O6 109.9(3) . . ? O1 S1 C7 104.1(2) . . ? O1 S1 C4 101.9(2) . . ? C7 S1 C4 99.4(3) . . ? O8 S5 C3 106.1(3) . . ? O8 S5 C8 106.7(3) . . ? C3 S5 C8 99.1(3) . . ? S1 O1 Cu1 120.91(17) . . ? S2 O2 Cu1 117.81(18) . . ? S3 O3 Cu1 116.45(17) . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.884 _refine_diff_density_max 0.615 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.077 #===END