Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Veciana, Jaume' 'Rovira, Concepcio' 'Ruiz-Molina, Daniel' 'Maspoch, Daniel' 'Wurst, Klaus' _publ_contact_author_name 'Prof Jaume Veciana' _publ_contact_author_address ; Prof Jaume Veciana Institut Ciencia Materials Barcelona (CSIC) Campus Universitari Bellaterra Cerdanyola Barcelona E-08193 SPAIN ; _publ_contact_author_email 'vecianaj@icmab.es' _publ_section_title ; A very Bulky Carboxylic Polychlorotriphenylmethyl Radical as a Novel Ligand for Transition Metal Complexes. A New Spin Frustated Metal System. ; data_1 _database_code_CSD 186141 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44 H30 Cl28 Cu O15' _chemical_formula_weight 1854.82 _chemical_melting_point ? _chemical_compound_source ? 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' '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 25.644(4) _cell_length_b 15.118(3) _cell_length_c 18.580(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.18(1) _cell_angle_gamma 90.00 _cell_volume 7198.0(22) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 46255 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method ? _exptl_crystal_F_000 3676 _exptl_absorpt_coefficient_mu 1.399 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Kappa CCD' _diffrn_measurement_method phi-scan _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9744 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 19.00 _reflns_number_total 4617 _reflns_number_observed 3134 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; poor crystal quality with high mosaicity and week diffraction (small crystal size). The Cu(H2O)3-unit is 5:1 disordered. The major part coordinates with O1 and O3, the minor with O2 and O4. The solvent molcules water and ethanol forming a network with hydrogen bonds. Six water and two ethanol were found and refined isotropically with occupancy of 0.833. Because of the disorder some of the solvents have bigger thermal parameters and the occupation could be lower than 0.833. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+62.1514P] 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 'not refined' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4212 _refine_ls_number_parameters 754 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1159 _refine_ls_R_factor_obs 0.0707 _refine_ls_wR_factor_all 0.2068 _refine_ls_wR_factor_obs 0.1678 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.150 _refine_ls_restrained_S_all 1.122 _refine_ls_restrained_S_obs 1.151 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cl1 Cl 1.1669(2) 0.5043(3) 0.8763(3) 0.076(2) Uani 1 d . . Cl2 Cl 1.2847(2) 0.5161(3) 0.8508(3) 0.0654(14) Uani 1 d . . Cl3 Cl 1.3056(2) 0.1734(3) 0.9317(3) 0.0664(14) Uani 1 d . . Cl4 Cl 1.1883(2) 0.1707(4) 0.9635(4) 0.126(3) Uani 1 d . . Cl5 Cl 1.3314(2) 0.4288(3) 1.0362(2) 0.0705(15) Uani 1 d . . Cl6 Cl 1.4021(2) 0.3621(3) 1.1607(3) 0.076(2) Uani 1 d . . Cl7 Cl 1.4953(2) 0.2385(3) 1.1311(3) 0.087(2) Uani 1 d . . Cl8 Cl 1.5092(2) 0.1637(3) 0.9771(3) 0.077(2) Uani 1 d . . Cl9 Cl 1.4365(2) 0.2230(3) 0.8511(2) 0.0552(13) Uani 1 d . . Cl10 Cl 1.4351(2) 0.4903(3) 0.9036(2) 0.0595(14) Uani 1 d . . Cl11 Cl 1.4872(2) 0.5476(3) 0.7656(3) 0.086(2) Uani 1 d . . Cl12 Cl 1.4419(2) 0.4867(4) 0.6176(3) 0.103(2) Uani 1 d . . Cl13 Cl 1.3443(2) 0.3651(3) 0.6077(3) 0.082(2) Uani 1 d . . Cl14 Cl 1.3026(2) 0.2827(3) 0.7452(2) 0.073(2) Uani 1 d . . Cl15 Cl 0.8646(2) 0.4151(4) 0.9270(3) 0.105(2) Uani 1 d . . Cl16 Cl 0.7498(2) 0.3857(3) 0.9652(2) 0.0586(13) Uani 1 d . . Cl17 Cl 0.7923(2) 0.0424(3) 1.0176(3) 0.083(2) Uani 1 d . . Cl18 Cl 0.9074(2) 0.0750(5) 0.9856(4) 0.137(3) Uani 1 d . . Cl19 Cl 0.7799(2) 0.2764(3) 1.1382(2) 0.0630(14) Uani 1 d . . Cl20 Cl 0.7663(2) 0.1808(3) 1.2808(2) 0.0709(15) Uani 1 d . . Cl21 Cl 0.6802(2) 0.0403(3) 1.2955(3) 0.083(2) Uani 1 d . . Cl22 Cl 0.6109(2) -0.0135(3) 1.1618(3) 0.080(2) Uani 1 d . . Cl23 Cl 0.6358(2) 0.0556(3) 1.0125(2) 0.0629(14) Uani 1 d . . Cl24 Cl 0.6330(2) 0.3207(3) 1.0541(2) 0.0600(14) Uani 1 d . . Cl25 Cl 0.5550(2) 0.3871(3) 0.9353(3) 0.0671(14) Uani 1 d . . Cl26 Cl 0.5611(2) 0.3169(3) 0.7797(3) 0.079(2) Uani 1 d . . Cl27 Cl 0.6427(2) 0.1753(3) 0.7426(2) 0.0712(15) Uani 1 d . . Cl28 Cl 0.7219(2) 0.1090(3) 0.8594(2) 0.0666(14) Uani 1 d . . O1 O 1.1020(5) 0.3082(10) 0.8759(11) 0.108(5) Uani 1 d . . O2 O 1.1089(6) 0.3495(12) 0.9891(11) 0.126(7) Uani 1 d . . O3 O 0.9517(7) 0.2538(12) 0.8848(11) 0.131(7) Uani 1 d . . O4 O 0.9623(7) 0.2830(14) 0.9997(13) 0.161(8) Uani 1 d . . C1 C 1.1266(9) 0.3342(15) 0.9311(16) 0.079(7) Uani 1 d . . C2 C 1.1848(7) 0.3363(15) 0.9194(9) 0.060(6) Uani 1 d . . C3 C 1.2060(7) 0.4131(12) 0.8932(9) 0.048(5) Uani 1 d . . C4 C 1.2585(7) 0.4190(11) 0.8829(9) 0.046(5) Uani 1 d . . C5 C 1.2927(6) 0.3475(12) 0.8962(8) 0.043(5) Uani 1 d . . C6 C 1.2691(7) 0.2696(11) 0.9216(9) 0.049(5) Uani 1 d . . C7 C 1.2177(8) 0.2639(11) 0.9333(10) 0.061(5) Uani 1 d . . C8 C 1.3500(6) 0.3517(10) 0.8893(10) 0.039(4) Uani 1 d . . C9 C 1.3846(6) 0.3207(11) 0.9487(11) 0.038(4) Uani 1 d . . C10 C 1.3788(6) 0.3520(11) 1.0174(14) 0.057(5) Uani 1 d . . C11 C 1.4113(8) 0.3242(12) 1.0742(10) 0.054(5) Uani 1 d . . C12 C 1.4525(8) 0.2717(14) 1.0623(11) 0.059(5) Uani 1 d . . C13 C 1.4596(6) 0.2383(11) 0.9937(15) 0.056(5) Uani 1 d . . C14 C 1.4274(7) 0.2638(10) 0.9361(10) 0.046(5) Uani 1 d . . C15 C 1.3706(6) 0.3844(10) 0.8218(12) 0.041(5) Uani 1 d . . C16 C 1.4124(6) 0.4448(11) 0.8241(9) 0.038(4) Uani 1 d . . C17 C 1.4347(6) 0.4758(10) 0.7626(13) 0.047(5) Uani 1 d . . C18 C 1.4143(8) 0.4492(13) 0.6959(12) 0.060(6) Uani 1 d . . C19 C 1.3714(8) 0.3946(13) 0.6908(10) 0.056(5) Uani 1 d . . C20 C 1.3511(6) 0.3622(11) 0.7524(13) 0.049(5) Uani 1 d . . C21 C 0.9374(10) 0.2603(21) 0.9471(19) 0.117(10) Uani 1 d . . C22 C 0.8782(8) 0.2421(20) 0.9580(11) 0.083(7) Uani 1 d . . C23 C 0.8433(9) 0.3117(13) 0.9511(10) 0.069(6) Uani 1 d . . C24 C 0.7916(7) 0.2961(13) 0.9659(8) 0.048(5) Uani 1 d . . C25 C 0.7755(6) 0.2124(14) 0.9873(8) 0.042(5) Uani 1 d . . C26 C 0.8110(7) 0.1448(12) 0.9941(9) 0.051(5) Uani 1 d . . C27 C 0.8619(8) 0.1590(14) 0.9812(11) 0.073(6) Uani 1 d . . C28 C 0.7195(6) 0.1982(10) 1.0060(10) 0.039(4) Uani 1 d . . C29 C 0.7077(6) 0.1622(10) 1.0777(10) 0.037(4) Uani 1 d . . C30 C 0.7365(6) 0.1877(10) 1.1390(12) 0.043(5) Uani 1 d . . C31 C 0.7294(6) 0.1529(13) 1.2054(11) 0.052(5) Uani 1 d . . C32 C 0.6904(8) 0.0877(12) 1.2130(10) 0.058(5) Uani 1 d . . C33 C 0.6607(6) 0.0632(9) 1.1513(13) 0.044(5) Uani 1 d . . C34 C 0.6694(6) 0.0989(11) 1.0849(10) 0.042(4) Uani 1 d . . C35 C 0.6778(6) 0.2229(11) 0.9526(11) 0.044(5) Uani 1 d . . C36 C 0.6366(7) 0.2803(11) 0.9663(9) 0.047(5) Uani 1 d . . C37 C 0.6017(6) 0.3108(11) 0.9144(12) 0.052(5) Uani 1 d . . C38 C 0.6065(7) 0.2765(13) 0.8440(10) 0.048(5) Uani 1 d . . C39 C 0.6420(8) 0.2148(11) 0.8292(10) 0.050(5) Uani 1 d . . C40 C 0.6786(6) 0.1910(11) 0.8819(12) 0.045(5) Uani 1 d . . Cu1 Cu 1.02733(10) 0.2789(3) 0.8765(2) 0.1157(14) Uani 0.83 d P 1 O5 O 1.0254(8) 0.2419(21) 0.7655(14) 0.225(13) Uani 0.83 d P 1 O6 O 1.0108(6) 0.4069(16) 0.8578(16) 0.194(12) Uani 0.83 d P 1 O7 O 1.0469(6) 0.1543(11) 0.9201(11) 0.125(7) Uani 0.83 d P 1 O8 O 1.0417(10) 0.1363(18) 1.0575(15) 0.192(10) Uiso 0.83 d P 1 O9 O 1.0009(13) 0.0108(20) 0.8579(17) 0.241(13) Uiso 0.83 d P 1 O10 O 0.9195(23) 0.4166(35) 0.7203(30) 0.442(30) Uiso 0.83 d P 1 O11 O 0.9071(16) 0.1279(25) 0.7682(22) 0.304(17) Uiso 0.83 d P 1 O12 O 0.9322(30) 0.1952(44) 0.6506(41) 0.549(42) Uiso 0.83 d P 1 O13 O 1.0016(42) 0.4565(63) 1.0690(48) 0.683(64) Uiso 0.83 d P 1 O14 O 1.1523(15) 0.1460(22) 0.6247(20) 0.270(15) Uiso 0.83 d PD 1 C41 C 1.2043(18) 0.1267(33) 0.6584(28) 0.248(22) Uiso 0.83 d PD 1 C42 C 1.2008(24) 0.1128(38) 0.7362(30) 0.297(28) Uiso 0.83 d PD 1 O15 O 1.1101(13) 0.3140(22) 0.6700(17) 0.241(13) Uiso 0.83 d PD 1 C43 C 1.1404(19) 0.3815(31) 0.7032(26) 0.256(23) Uiso 0.83 d PD 1 C44 C 1.1789(15) 0.4234(23) 0.6646(19) 0.162(13) Uiso 0.83 d PD 1 Cu1A Cu 1.0361(6) 0.3410(18) 1.0071(12) 0.164(10) Uani 0.17 d P 2 O5A O 1.0471(45) 0.3941(73) 1.1144(63) 0.159(40) Uiso 0.17 d P 2 O6A O 1.0220(24) 0.4659(42) 0.9674(37) 0.061(19) Uiso 0.17 d P 2 O7A O 1.0510(33) 0.1930(59) 1.0150(52) 0.104(28) Uiso 0.17 d P 2 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 Cl1 0.050(3) 0.066(4) 0.113(5) 0.008(3) -0.001(3) 0.009(3) Cl2 0.058(3) 0.036(3) 0.103(4) 0.010(3) 0.011(3) -0.004(2) Cl3 0.064(3) 0.045(3) 0.091(4) 0.013(3) 0.003(3) 0.003(2) Cl4 0.079(4) 0.079(4) 0.223(8) 0.067(5) 0.046(4) -0.002(3) Cl5 0.065(3) 0.082(4) 0.065(4) -0.023(3) 0.001(2) 0.026(3) Cl6 0.078(3) 0.102(4) 0.049(4) -0.017(3) -0.005(3) 0.002(3) Cl7 0.084(4) 0.097(4) 0.079(4) 0.006(3) -0.028(3) 0.016(3) Cl8 0.065(3) 0.064(4) 0.101(4) 0.007(3) 0.007(3) 0.024(3) Cl9 0.070(3) 0.043(3) 0.054(4) -0.012(2) 0.015(2) 0.006(2) Cl10 0.057(3) 0.045(3) 0.076(4) -0.015(3) -0.002(2) -0.003(2) Cl11 0.067(3) 0.066(4) 0.127(5) 0.014(3) 0.023(3) -0.018(3) Cl12 0.103(4) 0.120(5) 0.087(5) 0.055(4) 0.023(3) 0.004(4) Cl13 0.113(4) 0.086(4) 0.046(4) 0.007(3) 0.003(3) 0.010(3) Cl14 0.075(3) 0.086(4) 0.058(4) -0.017(3) -0.002(3) -0.027(3) Cl15 0.092(4) 0.101(5) 0.122(5) 0.019(4) 0.014(3) -0.049(4) Cl16 0.073(3) 0.042(3) 0.061(3) 0.007(2) 0.001(2) -0.003(2) Cl17 0.086(4) 0.056(4) 0.108(5) 0.017(3) 0.018(3) 0.020(3) Cl18 0.069(4) 0.145(6) 0.198(8) 0.026(5) 0.021(4) 0.044(4) Cl19 0.078(3) 0.059(3) 0.052(3) -0.001(3) -0.006(2) -0.020(3) Cl20 0.090(3) 0.076(4) 0.047(3) 0.005(3) -0.003(3) -0.002(3) Cl21 0.115(4) 0.074(4) 0.060(4) 0.018(3) 0.014(3) -0.011(3) Cl22 0.102(4) 0.068(4) 0.071(4) 0.004(3) 0.020(3) -0.035(3) Cl23 0.077(3) 0.062(3) 0.050(3) -0.006(3) 0.001(2) -0.022(3) Cl24 0.077(3) 0.061(3) 0.042(3) -0.015(2) 0.002(2) 0.020(3) Cl25 0.059(3) 0.069(3) 0.073(4) -0.001(3) -0.004(2) 0.018(3) Cl26 0.077(3) 0.098(4) 0.059(4) 0.010(3) -0.023(3) 0.002(3) Cl27 0.098(4) 0.081(4) 0.035(4) -0.012(3) 0.003(3) -0.017(3) Cl28 0.081(3) 0.054(3) 0.065(4) -0.013(3) 0.015(3) 0.011(3) O1 0.051(9) 0.116(13) 0.158(18) 0.015(12) 0.015(10) -0.016(9) O2 0.086(12) 0.151(16) 0.145(18) 0.016(13) 0.055(12) 0.010(10) O3 0.099(12) 0.178(17) 0.116(17) 0.028(14) 0.027(12) -0.045(11) O4 0.068(12) 0.229(22) 0.184(23) -0.006(17) -0.003(13) -0.019(13) C1 0.055(20) 0.086(18) 0.095(25) 0.014(17) -0.013(16) -0.015(13) C2 0.042(14) 0.076(17) 0.065(15) 0.020(12) 0.027(10) -0.017(13) C3 0.041(13) 0.047(14) 0.057(13) 0.002(10) 0.003(9) 0.022(11) C4 0.051(13) 0.031(13) 0.056(13) -0.005(9) -0.008(9) 0.011(11) C5 0.058(14) 0.040(14) 0.029(12) 0.000(9) -0.007(9) -0.015(12) C6 0.046(13) 0.035(13) 0.065(14) 0.013(10) -0.008(9) 0.011(11) C7 0.046(13) 0.038(14) 0.101(17) 0.016(11) 0.023(11) 0.008(11) C8 0.031(12) 0.049(12) 0.037(14) -0.009(10) 0.010(10) -0.007(9) C9 0.030(11) 0.043(12) 0.042(16) -0.010(11) 0.007(10) -0.011(10) C10 0.045(12) 0.059(14) 0.067(18) -0.024(13) 0.012(12) 0.008(10) C11 0.044(12) 0.068(14) 0.049(16) -0.014(12) 0.005(12) -0.006(11) C12 0.056(14) 0.092(17) 0.028(15) 0.018(12) -0.016(10) -0.017(13) C13 0.033(11) 0.056(14) 0.079(19) 0.023(13) -0.007(11) 0.006(9) C14 0.037(11) 0.020(11) 0.083(17) -0.010(11) 0.022(12) -0.012(9) C15 0.020(10) 0.018(11) 0.086(21) 0.005(11) 0.016(12) 0.000(8) C16 0.055(12) 0.045(12) 0.014(13) -0.005(10) 0.009(9) 0.013(10) C17 0.050(11) 0.039(13) 0.053(17) -0.009(12) 0.008(12) 0.013(9) C18 0.073(14) 0.054(15) 0.056(19) 0.043(13) 0.027(13) 0.007(12) C19 0.090(16) 0.050(14) 0.026(16) 0.001(11) 0.001(12) 0.021(12) C20 0.057(12) 0.057(14) 0.032(16) -0.002(12) -0.011(11) -0.002(10) C21 0.072(25) 0.174(29) 0.103(31) 0.035(24) -0.022(18) -0.017(18) C22 0.047(16) 0.128(24) 0.074(17) 0.012(15) -0.001(11) 0.003(17) C23 0.066(16) 0.064(16) 0.077(16) 0.015(12) -0.004(12) -0.012(14) C24 0.046(13) 0.062(16) 0.037(13) 0.014(10) 0.021(9) 0.004(11) C25 0.043(13) 0.069(16) 0.015(11) 0.003(10) -0.005(8) 0.003(13) C26 0.035(13) 0.064(16) 0.055(13) 0.010(10) -0.001(9) 0.010(12) C27 0.043(15) 0.060(16) 0.118(19) 0.028(13) 0.005(12) 0.021(12) C28 0.036(12) 0.043(12) 0.036(15) -0.001(10) -0.010(10) 0.002(9) C29 0.053(12) 0.027(12) 0.029(15) -0.003(11) -0.008(11) 0.013(10) C30 0.053(11) 0.053(13) 0.025(15) 0.015(12) 0.012(11) 0.004(9) C31 0.035(10) 0.066(15) 0.054(18) -0.009(12) -0.007(9) 0.001(10) C32 0.074(14) 0.049(14) 0.050(17) 0.014(12) 0.013(12) 0.010(12) C33 0.066(12) 0.014(11) 0.054(17) 0.006(11) 0.013(12) -0.004(9) C34 0.056(12) 0.026(12) 0.044(16) 0.003(11) 0.002(10) -0.011(10) C35 0.053(13) 0.036(12) 0.044(16) -0.009(11) 0.015(11) -0.005(10) C36 0.057(12) 0.038(12) 0.049(14) -0.001(10) 0.024(11) 0.012(10) C37 0.029(10) 0.055(13) 0.072(17) 0.005(13) -0.010(10) 0.014(9) C38 0.072(14) 0.051(14) 0.021(15) -0.003(11) -0.007(10) -0.025(11) C39 0.077(14) 0.025(12) 0.049(16) -0.001(11) 0.015(13) -0.004(11) C40 0.046(11) 0.049(13) 0.041(15) 0.000(11) 0.011(10) 0.002(9) Cu1 0.036(2) 0.169(4) 0.144(4) 0.023(3) 0.020(2) -0.020(2) O5 0.096(15) 0.406(42) 0.172(25) 0.008(24) -0.015(15) -0.081(21) O6 0.051(11) 0.211(24) 0.321(34) 0.145(23) 0.001(15) 0.012(13) O7 0.066(11) 0.107(15) 0.202(22) 0.014(13) 0.018(12) -0.020(10) Cu1A 0.030(9) 0.284(29) 0.179(22) 0.077(20) 0.012(11) -0.036(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 Cl1 C3 1.73(2) . ? Cl2 C4 1.73(2) . ? Cl3 C6 1.74(2) . ? Cl4 C7 1.70(2) . ? Cl5 C10 1.73(2) . ? Cl6 C11 1.73(2) . ? Cl7 C12 1.73(2) . ? Cl8 C13 1.74(2) . ? Cl9 C14 1.72(2) . ? Cl10 C16 1.71(2) . ? Cl11 C17 1.73(2) . ? Cl12 C18 1.74(2) . ? Cl13 C19 1.73(2) . ? Cl14 C20 1.73(2) . ? Cl15 C23 1.72(2) . ? Cl16 C24 1.73(2) . ? Cl17 C26 1.68(2) . ? Cl18 C27 1.72(2) . ? Cl19 C30 1.74(2) . ? Cl20 C31 1.71(2) . ? Cl21 C32 1.72(2) . ? Cl22 C33 1.74(2) . ? Cl23 C34 1.70(2) . ? Cl24 C36 1.75(2) . ? Cl25 C37 1.72(2) . ? Cl26 C38 1.75(2) . ? Cl27 C39 1.72(2) . ? Cl28 C40 1.73(2) . ? O1 C1 1.25(2) . ? O1 Cu1 1.967(14) . ? O2 C1 1.21(2) . ? O2 Cu1A 1.91(2) . ? O3 C21 1.23(3) . ? O3 Cu1 1.99(2) . ? O4 C21 1.20(3) . ? O4 Cu1A 2.09(2) . ? C1 C2 1.52(3) . ? C2 C3 1.38(2) . ? C2 C7 1.40(2) . ? C3 C4 1.37(2) . ? C4 C5 1.41(2) . ? C5 C6 1.41(2) . ? C5 C8 1.48(2) . ? C6 C7 1.35(2) . ? C8 C15 1.47(2) . ? C8 C9 1.47(2) . ? C9 C10 1.38(2) . ? C9 C14 1.42(2) . ? C10 C11 1.39(2) . ? C11 C12 1.34(2) . ? C12 C13 1.39(2) . ? C13 C14 1.38(2) . ? C15 C20 1.41(2) . ? C15 C16 1.41(2) . ? C16 C17 1.38(2) . ? C17 C18 1.39(2) . ? C18 C19 1.37(2) . ? C19 C20 1.37(2) . ? C21 C22 1.56(3) . ? C22 C23 1.38(3) . ? C22 C27 1.40(3) . ? C23 C24 1.39(2) . ? C24 C25 1.39(2) . ? C25 C26 1.37(2) . ? C25 C28 1.51(2) . ? C26 C27 1.35(2) . ? C28 C35 1.48(2) . ? C28 C29 1.48(2) . ? C29 C34 1.38(2) . ? C29 C30 1.39(2) . ? C30 C31 1.36(2) . ? C31 C32 1.41(2) . ? C32 C33 1.40(2) . ? C33 C34 1.37(2) . ? C35 C36 1.40(2) . ? C35 C40 1.40(2) . ? C36 C37 1.37(2) . ? C37 C38 1.42(2) . ? C38 C39 1.34(2) . ? C39 C40 1.38(2) . ? Cu1 O6 2.01(2) . ? Cu1 O7 2.10(2) . ? Cu1 O5 2.14(3) . ? O14 C41 1.48(3) . ? C41 C42 1.47(3) . ? O15 C43 1.41(3) . ? C43 C44 1.39(3) . ? Cu1A O6A 2.05(7) . ? Cu1A O5A 2.16(12) . ? Cu1A O7A 2.27(9) . ? 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 C1 O1 Cu1 121.8(17) . . ? C1 O2 Cu1A 123.0(20) . . ? C21 O3 Cu1 112.5(19) . . ? C21 O4 Cu1A 129.0(24) . . ? O2 C1 O1 126.9(24) . . ? O2 C1 C2 121.9(23) . . ? O1 C1 C2 111.0(24) . . ? C3 C2 C7 118.6(14) . . ? C3 C2 C1 118.2(20) . . ? C7 C2 C1 123.2(19) . . ? C4 C3 C2 120.5(15) . . ? C4 C3 Cl1 119.3(16) . . ? C2 C3 Cl1 120.1(15) . . ? C3 C4 C5 122.3(15) . . ? C3 C4 Cl2 120.1(14) . . ? C5 C4 Cl2 117.6(14) . . ? C4 C5 C6 115.2(14) . . ? C4 C5 C8 124.4(16) . . ? C6 C5 C8 120.3(17) . . ? C7 C6 C5 122.8(15) . . ? C7 C6 Cl3 117.1(15) . . ? C5 C6 Cl3 119.9(14) . . ? C6 C7 C2 120.5(15) . . ? C6 C7 Cl4 123.7(16) . . ? C2 C7 Cl4 115.8(14) . . ? C15 C8 C9 121.6(13) . . ? C15 C8 C5 118.7(14) . . ? C9 C8 C5 119.7(15) . . ? C10 C9 C14 118.3(16) . . ? C10 C9 C8 120.3(16) . . ? C14 C9 C8 121.3(17) . . ? C9 C10 C11 121.2(16) . . ? C9 C10 Cl5 121.4(17) . . ? C11 C10 Cl5 117.4(18) . . ? C12 C11 C10 120.6(16) . . ? C12 C11 Cl6 118.9(18) . . ? C10 C11 Cl6 120.4(17) . . ? C11 C12 C13 119.7(15) . . ? C11 C12 Cl7 122.1(20) . . ? C13 C12 Cl7 118.1(20) . . ? C14 C13 C12 120.9(16) . . ? C14 C13 Cl8 117.6(18) . . ? C12 C13 Cl8 121.5(18) . . ? C13 C14 C9 118.9(16) . . ? C13 C14 Cl9 120.9(15) . . ? C9 C14 Cl9 120.1(16) . . ? C20 C15 C16 115.2(15) . . ? C20 C15 C8 125.3(15) . . ? C16 C15 C8 119.5(17) . . ? C17 C16 C15 122.3(15) . . ? C17 C16 Cl10 116.1(15) . . ? C15 C16 Cl10 121.4(14) . . ? C16 C17 C18 119.2(16) . . ? C16 C17 Cl11 122.2(17) . . ? C18 C17 Cl11 118.6(18) . . ? C19 C18 C17 120.6(15) . . ? C19 C18 Cl12 119.3(20) . . ? C17 C18 Cl12 120.1(19) . . ? C20 C19 C18 119.1(16) . . ? C20 C19 Cl13 120.2(19) . . ? C18 C19 Cl13 120.7(19) . . ? C19 C20 C15 123.4(16) . . ? C19 C20 Cl14 118.6(17) . . ? C15 C20 Cl14 117.8(15) . . ? O4 C21 O3 128.5(30) . . ? O4 C21 C22 115.8(29) . . ? O3 C21 C22 115.6(25) . . ? C23 C22 C27 120.8(17) . . ? C23 C22 C21 118.8(24) . . ? C27 C22 C21 120.1(23) . . ? C22 C23 C24 118.2(17) . . ? C22 C23 Cl15 120.3(18) . . ? C24 C23 Cl15 121.5(18) . . ? C23 C24 C25 120.5(16) . . ? C23 C24 Cl16 117.6(17) . . ? C25 C24 Cl16 121.7(13) . . ? C26 C25 C24 120.0(14) . . ? C26 C25 C28 120.6(17) . . ? C24 C25 C28 119.3(16) . . ? C27 C26 C25 120.5(16) . . ? C27 C26 Cl17 118.5(16) . . ? C25 C26 Cl17 120.9(14) . . ? C26 C27 C22 119.9(16) . . ? C26 C27 Cl18 122.1(18) . . ? C22 C27 Cl18 117.9(17) . . ? C35 C28 C29 122.0(14) . . ? C35 C28 C25 118.7(15) . . ? C29 C28 C25 119.2(13) . . ? C34 C29 C30 118.1(15) . . ? C34 C29 C28 120.7(16) . . ? C30 C29 C28 121.1(16) . . ? C31 C30 C29 123.5(16) . . ? C31 C30 Cl19 114.5(16) . . ? C29 C30 Cl19 121.7(15) . . ? C30 C31 C32 118.7(15) . . ? C30 C31 Cl20 123.8(16) . . ? C32 C31 Cl20 117.4(18) . . ? C33 C32 C31 117.8(15) . . ? C33 C32 Cl21 121.5(17) . . ? C31 C32 Cl21 120.7(18) . . ? C34 C33 C32 122.0(15) . . ? C34 C33 Cl22 120.5(16) . . ? C32 C33 Cl22 117.5(16) . . ? C33 C34 C29 120.0(15) . . ? C33 C34 Cl23 117.7(15) . . ? C29 C34 Cl23 122.1(16) . . ? C36 C35 C40 114.9(15) . . ? C36 C35 C28 124.5(17) . . ? C40 C35 C28 120.5(16) . . ? C37 C36 C35 123.9(16) . . ? C37 C36 Cl24 118.9(15) . . ? C35 C36 Cl24 117.0(15) . . ? C36 C37 C38 116.7(15) . . ? C36 C37 Cl25 120.6(17) . . ? C38 C37 Cl25 122.7(16) . . ? C39 C38 C37 121.9(15) . . ? C39 C38 Cl26 122.9(17) . . ? C37 C38 Cl26 115.1(17) . . ? C38 C39 C40 119.0(16) . . ? C38 C39 Cl27 117.8(17) . . ? C40 C39 Cl27 123.0(17) . . ? C39 C40 C35 123.0(15) . . ? C39 C40 Cl28 116.2(16) . . ? C35 C40 Cl28 120.4(15) . . ? O1 Cu1 O3 175.4(9) . . ? O1 Cu1 O6 88.9(7) . . ? O3 Cu1 O6 89.8(7) . . ? O1 Cu1 O7 89.2(6) . . ? O3 Cu1 O7 91.1(7) . . ? O6 Cu1 O7 167.1(11) . . ? O1 Cu1 O5 92.3(8) . . ? O3 Cu1 O5 92.2(8) . . ? O6 Cu1 O5 95.1(12) . . ? O7 Cu1 O5 97.7(11) . . ? C42 C41 O14 110.9(46) . . ? C44 C43 O15 119.5(44) . . ? O2 Cu1A O6A 92.0(20) . . ? O2 Cu1A O4 154.9(18) . . ? O6A Cu1A O4 102.5(20) . . ? O2 Cu1A O5A 92.4(32) . . ? O6A Cu1A O5A 90.3(37) . . ? O4 Cu1A O5A 107.7(32) . . ? O2 Cu1A O7A 85.1(24) . . ? O6A Cu1A O7A 162.6(33) . . ? O4 Cu1A O7A 74.9(23) . . ? O5A Cu1A O7A 106.9(39) . . ? _refine_diff_density_max 0.561 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.081 #===END data_2 _database_code_CSD 186142 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H34 Cl28 Cu2 O14' _chemical_formula_weight 2002.47 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' '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 26.296(2) _cell_length_b 16.9040(9) _cell_length_c 8.5648(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.760(3) _cell_angle_gamma 90.00 _cell_volume 3798.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 32930 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 1.601 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Kappa CCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12387 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 19.75 _reflns_number_total 3413 _reflns_number_gt 2724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+23.3969P] 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, refined at O5 with bond restraints' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3413 _refine_ls_number_parameters 444 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.218 _refine_ls_restrained_S_all 1.217 _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 0.50003(5) 0.57035(7) 0.43187(14) 0.0396(4) Uani 1 1 d . . . O1 O 0.5745(3) 0.5663(4) 0.4760(8) 0.0510(19) Uani 1 1 d . . . O2 O 0.5743(3) 0.4435(5) 0.5800(8) 0.053(2) Uani 1 1 d . . . O3 O 0.5063(3) 0.5050(5) 0.2460(7) 0.054(2) Uani 1 1 d . . . O4 O 0.5054(3) 0.3862(4) 0.3589(8) 0.053(2) Uani 1 1 d . . . O5 O 0.4970(4) 0.6815(5) 0.3215(10) 0.060(2) Uani 1 1 d D . . H5A H 0.521(3) 0.693(7) 0.266(11) 0.08(5) Uiso 1 1 d D . . H5B H 0.473(4) 0.707(8) 0.273(16) 0.14(7) Uiso 1 1 d D . . C1 C 0.5952(4) 0.5060(8) 0.5350(12) 0.046(3) Uani 1 1 d . . . C2 C 0.6530(4) 0.5073(6) 0.5586(13) 0.041(3) Uani 1 1 d . . . C3 C 0.6770(4) 0.5272(6) 0.7018(11) 0.039(3) Uani 1 1 d . . . C4 C 0.7295(4) 0.5276(6) 0.7234(11) 0.040(3) Uani 1 1 d . . . C5 C 0.7605(4) 0.5070(6) 0.6019(12) 0.040(3) Uani 1 1 d . . . C6 C 0.7351(4) 0.4903(6) 0.4582(12) 0.044(3) Uani 1 1 d . . . C7 C 0.6823(4) 0.4896(6) 0.4383(12) 0.043(3) Uani 1 1 d . . . C8 C 0.8159(4) 0.5054(6) 0.6228(11) 0.043(3) Uani 1 1 d . . . C9 C 0.8434(4) 0.4366(6) 0.5742(12) 0.044(3) Uani 1 1 d . . . C10 C 0.8281(4) 0.3587(7) 0.6027(11) 0.044(3) Uani 1 1 d . . . C11 C 0.8551(5) 0.2940(6) 0.5573(13) 0.047(3) Uani 1 1 d . . . C12 C 0.8979(5) 0.3034(7) 0.4741(14) 0.055(3) Uani 1 1 d . . . C13 C 0.9129(4) 0.3798(7) 0.4411(12) 0.048(3) Uani 1 1 d . . . C14 C 0.8866(4) 0.4444(6) 0.4836(11) 0.040(3) Uani 1 1 d . . . C15 C 0.8445(4) 0.5720(6) 0.7000(12) 0.040(3) Uani 1 1 d . . . C16 C 0.8856(4) 0.5577(6) 0.8137(11) 0.036(3) Uani 1 1 d . . . C17 C 0.9152(4) 0.6181(6) 0.8712(11) 0.042(3) Uani 1 1 d . . . C18 C 0.9060(4) 0.6964(6) 0.8248(12) 0.045(3) Uani 1 1 d . . . C19 C 0.8636(4) 0.7120(6) 0.7232(12) 0.043(3) Uani 1 1 d . . . C20 C 0.8339(4) 0.6522(6) 0.6605(11) 0.039(3) Uani 1 1 d . . . C21 C 0.5070(4) 0.4308(7) 0.2406(14) 0.045(3) Uani 1 1 d . . . C22 C 0.5116(5) 0.3937(7) 0.0852(11) 0.076(4) Uani 1 1 d . . . H22A H 0.4797 0.3995 0.0228 0.114 Uiso 1 1 calc R . . H22B H 0.5195 0.3380 0.0987 0.114 Uiso 1 1 calc R . . H22C H 0.5387 0.4194 0.0326 0.114 Uiso 1 1 calc R . . Cl1 Cl 0.63903(10) 0.54927(18) 0.8539(3) 0.0614(9) Uani 1 1 d . . . Cl2 Cl 0.75658(11) 0.5463(2) 0.9087(3) 0.0687(10) Uani 1 1 d . . . Cl3 Cl 0.77016(11) 0.4738(2) 0.2946(3) 0.0667(9) Uani 1 1 d . . . Cl4 Cl 0.65247(11) 0.4662(2) 0.2561(3) 0.0697(9) Uani 1 1 d . . . Cl5 Cl 0.77765(12) 0.34275(18) 0.7194(4) 0.0690(9) Uani 1 1 d . . . Cl6 Cl 0.83582(13) 0.19945(17) 0.6046(4) 0.0779(10) Uani 1 1 d . . . Cl7 Cl 0.93107(13) 0.22359(18) 0.4151(4) 0.0832(11) Uani 1 1 d . . . Cl8 Cl 0.96596(12) 0.39123(19) 0.3286(4) 0.0806(10) Uani 1 1 d . . . Cl9 Cl 0.90463(11) 0.53632(16) 0.4221(4) 0.0636(9) Uani 1 1 d . . . Cl10 Cl 0.89449(11) 0.46504(15) 0.8897(3) 0.0610(9) Uani 1 1 d . . . Cl11 Cl 0.96453(10) 0.59937(16) 1.0092(3) 0.0605(8) Uani 1 1 d . . . Cl12 Cl 0.94382(12) 0.77184(17) 0.8979(4) 0.0717(10) Uani 1 1 d . . . Cl13 Cl 0.84978(12) 0.80917(15) 0.6702(4) 0.0660(9) Uani 1 1 d . . . Cl14 Cl 0.78543(11) 0.67485(17) 0.5216(3) 0.0641(9) Uani 1 1 d . . . O6 O 0.4197(4) 0.7568(5) 0.1503(12) 0.089(3) Uani 1 1 d . . . H6 H 0.4328 0.7997 0.1284 0.133 Uiso 1 1 calc R . . O7 O 0.5776(4) 0.7592(6) 0.2065(12) 0.112(4) Uani 1 1 d . . . H7 H 0.5552 0.7748 0.1409 0.168 Uiso 1 1 calc R . . C23 C 0.3757(9) 0.7452(13) 0.055(2) 0.146(8) Uani 1 1 d . . . H23A H 0.3585 0.7964 0.0429 0.176 Uiso 1 1 calc . . . H23B H 0.3861 0.7299 -0.0486 0.176 Uiso 1 1 calc . . . C24 C 0.3432(10) 0.696(2) 0.094(3) 0.245(16) Uani 1 1 d . . . H24A H 0.3152 0.6941 0.0142 0.368 Uiso 1 1 calc . . . H24B H 0.3305 0.7111 0.1930 0.368 Uiso 1 1 calc . . . H24C H 0.3588 0.6439 0.1035 0.368 Uiso 1 1 calc . . . C25 C 0.6166(10) 0.7283(18) 0.132(3) 0.219(14) Uani 1 1 d . . . H25A H 0.6037 0.6802 0.0795 0.263 Uiso 1 1 calc . . . H25B H 0.6243 0.7658 0.0499 0.263 Uiso 1 1 calc . . . C26 C 0.6588(9) 0.7102(15) 0.204(3) 0.191(11) Uani 1 1 d . . . H26A H 0.6816 0.6891 0.1294 0.286 Uiso 1 1 calc . . . H26B H 0.6531 0.6707 0.2826 0.286 Uiso 1 1 calc . . . H26C H 0.6739 0.7570 0.2530 0.286 Uiso 1 1 calc . . . 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 0.0466(8) 0.0349(7) 0.0371(8) 0.0038(6) 0.0002(6) 0.0011(6) O1 0.045(5) 0.048(5) 0.060(5) 0.013(4) 0.000(4) 0.002(4) O2 0.045(5) 0.049(5) 0.063(5) 0.012(4) 0.001(4) 0.003(4) O3 0.080(6) 0.047(6) 0.033(4) -0.002(4) 0.003(4) 0.012(4) O4 0.083(6) 0.040(5) 0.036(5) -0.003(4) 0.002(4) 0.006(4) O5 0.078(6) 0.046(5) 0.056(6) 0.022(4) 0.001(5) 0.000(5) C1 0.046(9) 0.071(10) 0.021(6) -0.006(6) -0.002(6) 0.009(8) C2 0.045(8) 0.037(7) 0.042(8) 0.004(5) 0.001(7) 0.004(5) C3 0.046(8) 0.044(7) 0.026(7) 0.000(5) 0.002(6) 0.007(5) C4 0.046(8) 0.038(7) 0.035(7) 0.002(5) -0.008(6) -0.003(5) C5 0.043(8) 0.049(7) 0.026(7) -0.013(5) 0.001(6) 0.000(5) C6 0.052(8) 0.049(7) 0.033(7) 0.015(6) 0.011(6) 0.007(6) C7 0.047(8) 0.048(7) 0.035(7) 0.000(5) -0.001(6) 0.000(6) C8 0.050(8) 0.037(7) 0.042(7) 0.014(6) 0.009(6) 0.003(6) C9 0.045(7) 0.046(8) 0.041(7) -0.001(6) -0.001(6) 0.007(6) C10 0.049(7) 0.043(8) 0.038(7) 0.007(6) -0.009(5) -0.006(6) C11 0.062(8) 0.026(7) 0.051(8) 0.003(6) -0.019(7) 0.000(6) C12 0.051(8) 0.048(9) 0.063(8) -0.006(6) -0.011(7) 0.018(7) C13 0.044(7) 0.049(8) 0.050(7) 0.001(6) 0.002(6) -0.001(7) C14 0.056(8) 0.024(7) 0.041(7) 0.000(5) 0.004(6) 0.010(6) C15 0.041(7) 0.027(7) 0.054(8) -0.004(6) 0.018(6) 0.009(6) C16 0.037(7) 0.032(7) 0.041(7) 0.006(5) 0.006(6) 0.000(5) C17 0.047(7) 0.042(8) 0.038(7) -0.003(6) 0.005(5) 0.002(6) C18 0.053(8) 0.042(8) 0.043(7) -0.006(6) 0.012(6) -0.001(6) C19 0.070(8) 0.026(7) 0.035(7) 0.000(5) 0.015(6) 0.011(6) C20 0.045(7) 0.048(8) 0.025(6) -0.007(6) 0.004(5) 0.005(6) C21 0.044(7) 0.036(8) 0.055(9) 0.005(7) 0.009(6) 0.004(6) C22 0.141(12) 0.068(9) 0.018(7) -0.006(6) 0.005(7) 0.009(8) Cl1 0.0559(19) 0.089(2) 0.0404(17) -0.0095(16) 0.0129(14) 0.0024(16) Cl2 0.0573(19) 0.115(3) 0.0335(17) -0.0088(17) -0.0009(14) -0.0077(18) Cl3 0.063(2) 0.101(3) 0.0373(17) -0.0020(17) 0.0096(15) 0.0206(18) Cl4 0.065(2) 0.101(3) 0.0415(18) -0.0173(17) -0.0121(15) 0.0054(18) Cl5 0.075(2) 0.059(2) 0.074(2) 0.0185(17) 0.0126(17) -0.0136(17) Cl6 0.103(3) 0.0374(18) 0.090(2) 0.0071(17) -0.020(2) -0.0117(17) Cl7 0.092(3) 0.047(2) 0.108(3) -0.0202(19) -0.014(2) 0.0239(18) Cl8 0.070(2) 0.070(2) 0.106(3) -0.009(2) 0.030(2) 0.0124(18) Cl9 0.070(2) 0.0410(17) 0.084(2) 0.0054(16) 0.0345(17) -0.0005(15) Cl10 0.071(2) 0.0367(17) 0.071(2) 0.0079(15) -0.0244(16) -0.0011(15) Cl11 0.0525(18) 0.0532(19) 0.074(2) -0.0051(16) -0.0103(15) -0.0050(15) Cl12 0.080(2) 0.0424(18) 0.093(3) -0.0119(17) 0.0068(19) -0.0146(16) Cl13 0.090(2) 0.0332(17) 0.076(2) 0.0062(15) 0.0197(18) 0.0082(15) Cl14 0.068(2) 0.0543(19) 0.068(2) 0.0191(16) -0.0062(16) 0.0115(16) O6 0.085(7) 0.078(7) 0.100(7) 0.029(6) -0.016(6) -0.015(5) O7 0.105(8) 0.090(8) 0.142(10) 0.049(7) 0.010(7) 0.007(6) C23 0.16(2) 0.19(2) 0.092(14) -0.017(13) 0.003(14) -0.073(16) C24 0.22(3) 0.37(4) 0.14(2) -0.02(2) 0.012(18) -0.20(3) C25 0.16(2) 0.36(4) 0.15(2) 0.00(2) 0.057(18) 0.15(2) C26 0.16(2) 0.23(3) 0.17(2) -0.087(19) 0.000(17) 0.10(2) _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 O4 1.950(7) 3_666 ? Cu1 O3 1.954(7) . ? Cu1 O2 1.964(7) 3_666 ? Cu1 O1 1.971(7) . ? Cu1 O5 2.102(8) . ? Cu1 Cu1 2.649(2) 3_666 ? O1 C1 1.247(12) . ? O2 C1 1.264(13) . ? O2 Cu1 1.964(7) 3_666 ? O3 C21 1.254(12) . ? O4 C21 1.267(12) . ? O4 Cu1 1.950(7) 3_666 ? C1 C2 1.521(14) . ? C2 C7 1.359(13) . ? C2 C3 1.384(13) . ? C3 C4 1.379(13) . ? C3 Cl1 1.734(10) . ? C4 C5 1.407(13) . ? C4 Cl2 1.726(10) . ? C5 C6 1.390(13) . ? C5 C8 1.459(13) . ? C6 C7 1.388(13) . ? C6 Cl3 1.750(10) . ? C7 Cl4 1.746(10) . ? C8 C9 1.444(14) . ? C8 C15 1.484(14) . ? C9 C10 1.404(14) . ? C9 C14 1.423(13) . ? C10 C11 1.373(14) . ? C10 Cl5 1.734(11) . ? C11 C12 1.382(15) . ? C11 Cl6 1.732(11) . ? C12 C13 1.385(15) . ? C12 Cl7 1.701(11) . ? C13 C14 1.356(13) . ? C13 Cl8 1.757(11) . ? C14 Cl9 1.717(10) . ? C15 C20 1.419(13) . ? C15 C16 1.428(13) . ? C16 C17 1.356(13) . ? C16 Cl10 1.706(10) . ? C17 C18 1.397(14) . ? C17 Cl11 1.727(10) . ? C18 C19 1.394(14) . ? C18 Cl12 1.712(11) . ? C19 C20 1.365(13) . ? C19 Cl13 1.735(10) . ? C20 Cl14 1.730(10) . ? C21 C22 1.483(14) . ? O6 C23 1.39(2) . ? O7 C25 1.35(2) . ? C23 C24 1.25(2) . ? C25 C26 1.27(3) . ? 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 O4 Cu1 O3 167.6(3) 3_666 . ? O4 Cu1 O2 87.7(3) 3_666 3_666 ? O3 Cu1 O2 91.5(3) . 3_666 ? O4 Cu1 O1 88.2(3) 3_666 . ? O3 Cu1 O1 90.1(3) . . ? O2 Cu1 O1 168.1(3) 3_666 . ? O4 Cu1 O5 94.2(3) 3_666 . ? O3 Cu1 O5 98.2(3) . . ? O2 Cu1 O5 94.3(4) 3_666 . ? O1 Cu1 O5 97.2(4) . . ? O4 Cu1 Cu1 86.0(2) 3_666 3_666 ? O3 Cu1 Cu1 81.6(2) . 3_666 ? O2 Cu1 Cu1 83.5(2) 3_666 3_666 ? O1 Cu1 Cu1 85.0(2) . 3_666 ? O5 Cu1 Cu1 177.8(3) . 3_666 ? C1 O1 Cu1 120.5(7) . . ? C1 O2 Cu1 122.4(7) . 3_666 ? C21 O3 Cu1 126.7(7) . . ? C21 O4 Cu1 121.3(7) . 3_666 ? O1 C1 O2 128.3(10) . . ? O1 C1 C2 116.6(11) . . ? O2 C1 C2 115.0(10) . . ? C7 C2 C3 118.5(9) . . ? C7 C2 C1 120.5(10) . . ? C3 C2 C1 121.0(10) . . ? C4 C3 C2 121.0(9) . . ? C4 C3 Cl1 121.2(8) . . ? C2 C3 Cl1 117.8(8) . . ? C3 C4 C5 121.4(9) . . ? C3 C4 Cl2 118.3(8) . . ? C5 C4 Cl2 120.1(8) . . ? C6 C5 C4 115.9(9) . . ? C6 C5 C8 121.5(9) . . ? C4 C5 C8 122.5(9) . . ? C7 C6 C5 121.9(9) . . ? C7 C6 Cl3 118.5(8) . . ? C5 C6 Cl3 119.6(8) . . ? C2 C7 C6 121.1(9) . . ? C2 C7 Cl4 119.0(8) . . ? C6 C7 Cl4 119.9(9) . . ? C9 C8 C5 119.6(9) . . ? C9 C8 C15 119.4(9) . . ? C5 C8 C15 120.9(9) . . ? C10 C9 C14 115.4(9) . . ? C10 C9 C8 123.5(10) . . ? C14 C9 C8 120.9(10) . . ? C11 C10 C9 122.6(10) . . ? C11 C10 Cl5 117.9(9) . . ? C9 C10 Cl5 119.0(9) . . ? C10 C11 C12 120.5(10) . . ? C10 C11 Cl6 120.3(10) . . ? C12 C11 Cl6 119.2(10) . . ? C11 C12 C13 117.7(10) . . ? C11 C12 Cl7 120.9(10) . . ? C13 C12 Cl7 121.4(10) . . ? C14 C13 C12 122.6(10) . . ? C14 C13 Cl8 119.8(9) . . ? C12 C13 Cl8 117.4(9) . . ? C13 C14 C9 120.8(9) . . ? C13 C14 Cl9 119.3(9) . . ? C9 C14 Cl9 119.8(8) . . ? C20 C15 C16 116.8(9) . . ? C20 C15 C8 122.2(9) . . ? C16 C15 C8 120.9(9) . . ? C17 C16 C15 120.7(9) . . ? C17 C16 Cl10 119.5(8) . . ? C15 C16 Cl10 119.6(8) . . ? C16 C17 C18 121.7(9) . . ? C16 C17 Cl11 119.8(8) . . ? C18 C17 Cl11 118.5(8) . . ? C19 C18 C17 118.3(9) . . ? C19 C18 Cl12 120.6(9) . . ? C17 C18 Cl12 121.0(9) . . ? C20 C19 C18 121.1(9) . . ? C20 C19 Cl13 119.7(9) . . ? C18 C19 Cl13 119.2(9) . . ? C19 C20 C15 121.1(9) . . ? C19 C20 Cl14 118.8(8) . . ? C15 C20 Cl14 119.9(8) . . ? O3 C21 O4 124.4(10) . . ? O3 C21 C22 117.3(10) . . ? O4 C21 C22 118.4(10) . . ? C24 C23 O6 120(2) . . ? C26 C25 O7 122(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 19.75 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.298 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.074