# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Fairlamb, Ian' _publ_contact_author_email ijsf1@york.ac.uk _publ_section_title ; Cu(I) complexes containing a multidentate and conformationally flexible dibenzylidene acetone ligand (dbathiophos): application in catalytic alkene cyclopropanation ; loop_ _publ_author_name A.Jarvis A.Whitwood I.Fairlamb # Attachment '- ijf0821m.cif' data_ijf0821m _database_code_depnum_ccdc_archive 'CCDC 801872' #TrackingRef '- ijf0821m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H32 O P2 S2, 2(C H2 Cl2)' _chemical_formula_sum 'C43 H36 Cl4 O P2 S2' _chemical_formula_weight 836.58 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.539(3) _cell_length_b 9.8002(10) _cell_length_c 17.1991(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.768(2) _cell_angle_gamma 90.00 _cell_volume 4135.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6151 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.498 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details 'SADABS v2.03 (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _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_% ? _diffrn_reflns_number 15724 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3666 _reflns_number_gt 3073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Considerable solvent disorder. 2 DCM Molecules modelled as disordered, each over two positions refined to relative occupancies 74:26 and 52:48 respectively. Atoms Cl4a Cl4b constrained to same position and same ADP. Atoms Cl1a Cl1b constrained to same position and same ADP.Atoms Cl2a Cl2b constrained to same position and same ADP. Atoms Cl3a Cl3b constrained to same position and same ADP. Atoms C23a C23b restrained as approximately isotropic. Further solvent disorder was evident but could not be modelled satisfactorily. ; _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^)+(0.0977P)^2^+15.8435P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3666 _refine_ls_number_parameters 268 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1732 _refine_ls_wR_factor_gt 0.1612 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.050 _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 C1 C 0.0000 0.4312(5) 0.2500 0.0324(11) Uani 1 2 d S . . C2 C 0.04207(13) 0.3508(4) 0.2096(2) 0.0329(8) Uani 1 1 d . . . H2 H 0.0395 0.2541 0.2097 0.039 Uiso 1 1 calc R . . C3 C 0.08316(13) 0.4094(3) 0.17332(18) 0.0261(7) Uani 1 1 d . . . H3 H 0.0841 0.5062 0.1717 0.031 Uiso 1 1 calc R . . C4 C 0.12721(13) 0.3349(3) 0.13551(17) 0.0246(7) Uani 1 1 d . . . C5 C 0.11644(14) 0.2070(3) 0.10301(19) 0.0298(7) Uani 1 1 d . . . H5 H 0.0801 0.1735 0.1018 0.036 Uiso 1 1 calc R . . C6 C 0.15804(15) 0.1279(3) 0.07235(19) 0.0307(7) Uani 1 1 d . . . H6 H 0.1500 0.0408 0.0508 0.037 Uiso 1 1 calc R . . C7 C 0.21065(14) 0.1757(3) 0.07330(18) 0.0287(7) Uani 1 1 d . . . H7 H 0.2392 0.1208 0.0535 0.034 Uiso 1 1 calc R . . C8 C 0.22212(13) 0.3048(3) 0.10339(17) 0.0242(7) Uani 1 1 d . . . H8 H 0.2585 0.3377 0.1035 0.029 Uiso 1 1 calc R . . C9 C 0.18090(12) 0.3860(3) 0.13324(16) 0.0216(6) Uani 1 1 d . . . C10 C 0.17537(12) 0.5697(3) 0.26557(17) 0.0226(6) Uani 1 1 d . . . C11 C 0.15195(13) 0.6904(3) 0.29133(19) 0.0269(7) Uani 1 1 d . . . H11 H 0.1477 0.7653 0.2567 0.032 Uiso 1 1 calc R . . C12 C 0.13470(14) 0.7019(4) 0.3678(2) 0.0324(8) Uani 1 1 d . . . H12 H 0.1188 0.7845 0.3853 0.039 Uiso 1 1 calc R . . C13 C 0.14078(14) 0.5928(4) 0.41804(19) 0.0337(8) Uani 1 1 d . . . H13 H 0.1290 0.6004 0.4703 0.040 Uiso 1 1 calc R . . C14 C 0.16405(15) 0.4725(4) 0.39233(19) 0.0328(8) Uani 1 1 d . . . H14 H 0.1683 0.3979 0.4272 0.039 Uiso 1 1 calc R . . C15 C 0.18124(14) 0.4599(3) 0.31614(18) 0.0278(7) Uani 1 1 d . . . H15 H 0.1969 0.3770 0.2987 0.033 Uiso 1 1 calc R . . C16 C 0.27028(13) 0.5725(3) 0.16376(18) 0.0238(7) Uani 1 1 d . . . C17 C 0.30272(14) 0.5405(3) 0.22859(18) 0.0273(7) Uani 1 1 d . . . H17 H 0.2862 0.5129 0.2757 0.033 Uiso 1 1 calc R . . C18 C 0.35892(14) 0.5488(4) 0.2244(2) 0.0315(8) Uani 1 1 d . . . H18 H 0.3807 0.5269 0.2687 0.038 Uiso 1 1 calc R . . C19 C 0.38357(14) 0.5889(3) 0.1561(2) 0.0316(7) Uani 1 1 d . . . H19 H 0.4222 0.5939 0.1534 0.038 Uiso 1 1 calc R . . C20 C 0.35164(14) 0.6215(3) 0.09202(19) 0.0295(7) Uani 1 1 d . . . H20 H 0.3685 0.6492 0.0452 0.035 Uiso 1 1 calc R . . C21 C 0.29543(14) 0.6144(3) 0.09533(18) 0.0277(7) Uani 1 1 d . . . H21 H 0.2739 0.6380 0.0510 0.033 Uiso 1 1 calc R . . O1 O 0.0000 0.5547(4) 0.2500 0.0457(10) Uani 1 2 d S . . P1 P 0.19651(3) 0.55973(8) 0.16492(4) 0.0215(2) Uani 1 1 d . . . S1 S 0.16234(4) 0.69891(8) 0.09835(5) 0.0307(3) Uani 1 1 d . . . C22A C 0.5181(4) 0.2971(11) 0.1551(8) 0.050(3) Uani 0.368(8) 1 d P A 1 H22A H 0.5560 0.2632 0.1605 0.04(3) Uiso 0.368(8) 1 calc PR A 1 H22B H 0.4939 0.2164 0.1518 0.09(5) Uiso 0.368(8) 1 calc PR A 1 Cl1A Cl 0.5000 0.4004(2) 0.2500 0.1215(12) Uani 0.736(15) 2 d SP . 1 Cl2A Cl 0.51210(10) 0.3921(3) 0.0633(2) 0.1628(13) Uani 0.368(8) 1 d P A 1 C22B C 0.5171(12) 0.438(3) 0.158(2) 0.050(3) Uani 0.132(8) 1 d P A 2 H22C H 0.5572 0.4452 0.1640 0.060 Uiso 0.132(8) 1 calc PR A 2 H22D H 0.5045 0.5336 0.1548 0.060 Uiso 0.132(8) 1 calc PR A 2 Cl1B Cl 0.5000 0.4004(2) 0.2500 0.1215(12) Uani 0.264(15) 2 d SP . 2 Cl2B Cl 0.51210(10) 0.3921(3) 0.0633(2) 0.1628(13) Uani 0.132(8) 1 d P A 2 C23A C 0.5105(5) 0.2539(15) -0.0038(8) 0.035(4) Uani 0.262(11) 1 d PU B 3 H23A H 0.4775 0.2730 -0.0359 0.042 Uiso 0.262(11) 1 calc PR B 3 H23B H 0.5416 0.2734 -0.0382 0.042 Uiso 0.262(11) 1 calc PR B 3 Cl3A Cl 0.51210(10) 0.3921(3) 0.0633(2) 0.1628(13) Uani 0.262(11) 1 d P B 3 Cl4A Cl 0.51083(19) 0.0872(10) 0.0026(3) 0.208(6) Uani 0.262(11) 1 d P . 3 C23B C 0.5153(6) 0.218(2) 0.0774(10) 0.055(6) Uani 0.238(11) 1 d PU B 4 H23C H 0.4861 0.1970 0.1147 0.05(5) Uiso 0.238(11) 1 calc PR B 4 H23D H 0.5502 0.2017 0.1054 0.06(6) Uiso 0.238(11) 1 calc PR B 4 Cl3B Cl 0.51210(10) 0.3921(3) 0.0633(2) 0.1628(13) Uani 0.238(11) 1 d P B 4 Cl4B Cl 0.51083(19) 0.0872(10) 0.0026(3) 0.208(6) Uani 0.238(11) 1 d P . 4 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 C1 0.027(2) 0.029(3) 0.041(3) 0.000 0.006(2) 0.000 C2 0.0295(18) 0.0285(18) 0.041(2) -0.0013(15) 0.0067(15) 0.0021(14) C3 0.0276(16) 0.0268(16) 0.0238(15) -0.0015(13) 0.0001(13) 0.0006(13) C4 0.0289(16) 0.0279(16) 0.0170(14) 0.0014(12) 0.0015(12) 0.0007(13) C5 0.0344(18) 0.0295(17) 0.0256(16) -0.0001(13) 0.0028(13) -0.0052(14) C6 0.045(2) 0.0246(16) 0.0228(16) -0.0035(13) 0.0069(14) -0.0025(14) C7 0.0382(18) 0.0283(17) 0.0199(15) -0.0005(13) 0.0062(13) 0.0059(14) C8 0.0277(16) 0.0279(16) 0.0171(14) 0.0014(12) 0.0028(12) 0.0013(13) C9 0.0279(16) 0.0237(15) 0.0131(13) 0.0015(11) 0.0015(11) 0.0013(12) C10 0.0243(15) 0.0253(16) 0.0183(14) -0.0018(12) 0.0027(12) -0.0024(12) C11 0.0304(17) 0.0249(16) 0.0256(16) -0.0026(13) 0.0019(13) 0.0000(13) C12 0.0328(18) 0.0352(19) 0.0292(17) -0.0096(14) 0.0051(14) 0.0024(14) C13 0.0392(19) 0.042(2) 0.0204(16) -0.0078(14) 0.0080(14) -0.0072(15) C14 0.048(2) 0.0304(18) 0.0200(16) 0.0016(13) 0.0042(14) -0.0083(15) C15 0.0383(18) 0.0228(16) 0.0223(15) -0.0011(12) 0.0047(13) -0.0015(13) C16 0.0294(16) 0.0200(15) 0.0221(15) -0.0025(12) 0.0044(12) -0.0010(12) C17 0.0345(18) 0.0270(16) 0.0205(15) -0.0022(13) 0.0033(13) -0.0002(13) C18 0.0335(18) 0.0335(18) 0.0274(17) -0.0057(14) -0.0019(14) 0.0010(14) C19 0.0303(17) 0.0280(17) 0.0366(19) -0.0074(14) 0.0044(14) -0.0022(14) C20 0.0363(18) 0.0256(16) 0.0269(17) -0.0012(13) 0.0105(14) -0.0037(14) C21 0.0353(18) 0.0255(16) 0.0223(16) -0.0001(12) 0.0040(13) -0.0035(13) O1 0.036(2) 0.028(2) 0.073(3) 0.000 0.0210(19) 0.000 P1 0.0272(4) 0.0213(4) 0.0162(4) 0.0015(3) 0.0032(3) 0.0006(3) S1 0.0392(5) 0.0288(5) 0.0241(4) 0.0079(3) 0.0017(3) 0.0055(3) C22A 0.025(5) 0.042(6) 0.082(8) 0.026(5) -0.004(5) 0.007(4) Cl1A 0.0843(16) 0.0631(13) 0.215(4) 0.000 -0.0701(19) 0.000 Cl2A 0.1145(17) 0.160(2) 0.216(3) 0.111(2) 0.0510(18) 0.0318(16) C22B 0.025(5) 0.042(6) 0.082(8) 0.026(5) -0.004(5) 0.007(4) Cl1B 0.0843(16) 0.0631(13) 0.215(4) 0.000 -0.0701(19) 0.000 Cl2B 0.1145(17) 0.160(2) 0.216(3) 0.111(2) 0.0510(18) 0.0318(16) C23A 0.022(5) 0.041(5) 0.040(5) 0.019(4) -0.019(4) 0.009(4) Cl3A 0.1145(17) 0.160(2) 0.216(3) 0.111(2) 0.0510(18) 0.0318(16) Cl4A 0.074(3) 0.478(19) 0.071(2) -0.031(6) -0.017(2) 0.070(5) C23B 0.013(7) 0.104(14) 0.049(10) 0.051(9) 0.012(6) 0.020(7) Cl3B 0.1145(17) 0.160(2) 0.216(3) 0.111(2) 0.0510(18) 0.0318(16) Cl4B 0.074(3) 0.478(19) 0.071(2) -0.031(6) -0.017(2) 0.070(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 C1 O1 1.211(6) . ? C1 C2 1.479(4) . ? C1 C2 1.479(4) 2 ? C2 C3 1.324(5) . ? C2 H2 0.9500 . ? C3 C4 1.464(4) . ? C3 H3 0.9500 . ? C4 C5 1.396(5) . ? C4 C9 1.411(4) . ? C5 C6 1.391(5) . ? C5 H5 0.9500 . ? C6 C7 1.373(5) . ? C6 H6 0.9500 . ? C7 C8 1.394(5) . ? C7 H7 0.9500 . ? C8 C9 1.391(4) . ? C8 H8 0.9500 . ? C9 P1 1.826(3) . ? C10 C15 1.389(4) . ? C10 C11 1.391(4) . ? C10 P1 1.816(3) . ? C11 C12 1.391(5) . ? C11 H11 0.9500 . ? C12 C13 1.382(5) . ? C12 H12 0.9500 . ? C13 C14 1.386(5) . ? C13 H13 0.9500 . ? C14 C15 1.387(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.397(5) . ? C16 C21 1.398(4) . ? C16 P1 1.815(3) . ? C17 C18 1.384(5) . ? C17 H17 0.9500 . ? C18 C19 1.385(5) . ? C18 H18 0.9500 . ? C19 C20 1.382(5) . ? C19 H19 0.9500 . ? C20 C21 1.383(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? P1 S1 1.9619(11) . ? C22A Cl2A 1.836(12) . ? C22A Cl1A 1.977(14) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? Cl1A C22A 1.977(14) 2_655 ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C23A Cl4A 1.638(16) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? Cl4A Cl4A 1.792(19) 5_655 ? C23B H23C 0.9900 . ? C23B H23D 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 O1 C1 C2 122.2(2) . . ? O1 C1 C2 122.2(2) . 2 ? C2 C1 C2 115.7(4) . 2 ? C3 C2 C1 122.1(3) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C4 124.4(3) . . ? C2 C3 H3 117.8 . . ? C4 C3 H3 117.8 . . ? C5 C4 C9 118.7(3) . . ? C5 C4 C3 119.2(3) . . ? C9 C4 C3 122.0(3) . . ? C6 C5 C4 121.1(3) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C5 120.0(3) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 119.9(3) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C4 119.4(3) . . ? C8 C9 P1 119.5(2) . . ? C4 C9 P1 121.0(2) . . ? C15 C10 C11 119.9(3) . . ? C15 C10 P1 121.8(2) . . ? C11 C10 P1 118.3(2) . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 119.8(3) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.0(3) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 120.6(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C10 119.5(3) . . ? C14 C15 H15 120.2 . . ? C10 C15 H15 120.2 . . ? C17 C16 C21 119.0(3) . . ? C17 C16 P1 122.2(2) . . ? C21 C16 P1 118.8(2) . . ? C18 C17 C16 120.2(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.5(3) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 119.5(3) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.7(3) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C16 120.1(3) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? C16 P1 C10 107.72(14) . . ? C16 P1 C9 105.43(14) . . ? C10 P1 C9 105.84(13) . . ? C16 P1 S1 111.36(11) . . ? C10 P1 S1 113.18(11) . . ? C9 P1 S1 112.80(10) . . ? Cl2A C22A Cl1A 115.7(6) . . ? Cl2A C22A H22A 108.4 . . ? Cl1A C22A H22A 108.4 . . ? Cl2A C22A H22B 108.4 . . ? Cl1A C22A H22B 108.4 . . ? H22A C22A H22B 107.4 . . ? C22A Cl1A C22A 118.4(6) . 2_655 ? H22C C22B H22D 104.2 . . ? Cl4A C23A H23A 103.3 . . ? Cl4A C23A H23B 103.3 . . ? H23A C23A H23B 105.2 . . ? C23A Cl4A Cl4A 161.3(6) . 5_655 ? H23C C23B H23D 106.1 . . ? 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 O1 C1 C2 C3 2.3(4) . . . . ? C2 C1 C2 C3 -177.7(4) 2 . . . ? C1 C2 C3 C4 177.1(3) . . . . ? C2 C3 C4 C5 30.9(5) . . . . ? C2 C3 C4 C9 -146.8(3) . . . . ? C9 C4 C5 C6 3.2(5) . . . . ? C3 C4 C5 C6 -174.6(3) . . . . ? C4 C5 C6 C7 -0.5(5) . . . . ? C5 C6 C7 C8 -1.4(5) . . . . ? C6 C7 C8 C9 0.5(5) . . . . ? C7 C8 C9 C4 2.3(4) . . . . ? C7 C8 C9 P1 -175.1(2) . . . . ? C5 C4 C9 C8 -4.1(4) . . . . ? C3 C4 C9 C8 173.6(3) . . . . ? C5 C4 C9 P1 173.2(2) . . . . ? C3 C4 C9 P1 -9.0(4) . . . . ? C15 C10 C11 C12 0.4(5) . . . . ? P1 C10 C11 C12 179.4(3) . . . . ? C10 C11 C12 C13 -0.1(5) . . . . ? C11 C12 C13 C14 0.0(5) . . . . ? C12 C13 C14 C15 -0.2(5) . . . . ? C13 C14 C15 C10 0.5(5) . . . . ? C11 C10 C15 C14 -0.6(5) . . . . ? P1 C10 C15 C14 -179.5(3) . . . . ? C21 C16 C17 C18 -0.8(5) . . . . ? P1 C16 C17 C18 178.6(2) . . . . ? C16 C17 C18 C19 0.0(5) . . . . ? C17 C18 C19 C20 0.4(5) . . . . ? C18 C19 C20 C21 -0.1(5) . . . . ? C19 C20 C21 C16 -0.7(5) . . . . ? C17 C16 C21 C20 1.1(5) . . . . ? P1 C16 C21 C20 -178.3(2) . . . . ? C17 C16 P1 C10 22.5(3) . . . . ? C21 C16 P1 C10 -158.1(2) . . . . ? C17 C16 P1 C9 -90.1(3) . . . . ? C21 C16 P1 C9 89.2(3) . . . . ? C17 C16 P1 S1 147.2(2) . . . . ? C21 C16 P1 S1 -33.5(3) . . . . ? C15 C10 P1 C16 -76.1(3) . . . . ? C11 C10 P1 C16 105.0(3) . . . . ? C15 C10 P1 C9 36.3(3) . . . . ? C11 C10 P1 C9 -142.6(2) . . . . ? C15 C10 P1 S1 160.4(2) . . . . ? C11 C10 P1 S1 -18.6(3) . . . . ? C8 C9 P1 C16 -9.9(3) . . . . ? C4 C9 P1 C16 172.8(2) . . . . ? C8 C9 P1 C10 -123.9(2) . . . . ? C4 C9 P1 C10 58.8(3) . . . . ? C8 C9 P1 S1 111.9(2) . . . . ? C4 C9 P1 S1 -65.4(2) . . . . ? Cl2A C22A Cl1A C22A 160.4(7) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.997 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.090 # Attachment '- ijf0825m.cif' data_ijf0825m _database_code_depnum_ccdc_archive 'CCDC 801873' #TrackingRef '- ijf0825m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H64 Cl2 Cu4 O2 P4 S4, 2(F6 P), 1.58(C4 H10 O), 0.41(C1 H2 Cl2)' _chemical_formula_sum 'C88.76 H80.42 Cl2.82 Cu4 F12 O3.59 P6 S4' _chemical_formula_weight 2117.11 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cu Cu 0.3201 1.2651 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0204(7) _cell_length_b 14.5437(9) _cell_length_c 15.1233(9) _cell_angle_alpha 71.9420(10) _cell_angle_beta 71.2710(10) _cell_angle_gamma 66.5850(10) _cell_volume 2246.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7178 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.32 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1067.7 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details 'SADABS v2.10; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _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_% ? _diffrn_reflns_number 23138 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.33 _reflns_number_total 11056 _reflns_number_gt 8605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The crystals contained a mixture of disordered solvents. Relative occupancy of each solvent was allowed to refine; overall occupancy was restrained to be 1.0. The solvents were modelled as an ether (79.4%) [with one terminal carbon disordered over two sites (C42 and C42a)] and a dichloromethane disordered over two sites (7.2% and 13.4%). All solvent atoms were modelled isotropically. Within the solvents, C-C bonds were restrained to be 1.51 angstroms, C-O bonds to 1.425 angstroms and C-Cl to 1.728 angstroms. ; _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^)+(0.0673P)^2^+3.1607P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11056 _refine_ls_number_parameters 571 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.046 _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 C1 C 0.7294(3) 0.1556(2) 0.2274(2) 0.0203(6) Uani 1 1 d . . . C2 C 0.7482(3) 0.1310(3) 0.1405(2) 0.0258(6) Uani 1 1 d . . . H2 H 0.7189 0.0801 0.1385 0.031 Uiso 1 1 calc R . . C3 C 0.8098(3) 0.1807(3) 0.0570(2) 0.0315(7) Uani 1 1 d . . . H3 H 0.8250 0.1619 -0.0016 0.038 Uiso 1 1 calc R . . C4 C 0.8492(3) 0.2575(3) 0.0586(2) 0.0318(7) Uani 1 1 d . . . H4 H 0.8879 0.2934 0.0008 0.038 Uiso 1 1 calc R . . C5 C 0.8321(3) 0.2821(3) 0.1448(2) 0.0264(7) Uani 1 1 d . . . H5 H 0.8605 0.3342 0.1455 0.032 Uiso 1 1 calc R . . C6 C 0.7736(3) 0.2312(2) 0.2306(2) 0.0201(6) Uani 1 1 d . . . C7 C 0.7674(3) 0.2497(2) 0.3232(2) 0.0187(6) Uani 1 1 d . . . C8 C 0.7611(3) 0.3392(2) 0.3402(2) 0.0188(6) Uani 1 1 d . . . C9 C 0.7900(3) 0.3337(2) 0.4311(2) 0.0189(6) Uani 1 1 d . . . C10 C 0.7715(3) 0.4334(2) 0.4510(2) 0.0179(5) Uani 1 1 d . . . C11 C 0.7937(3) 0.4366(2) 0.5334(2) 0.0177(5) Uani 1 1 d . . . C12 C 0.8092(3) 0.5262(2) 0.5488(2) 0.0179(5) Uani 1 1 d . . . C13 C 0.7738(3) 0.5476(2) 0.6407(2) 0.0184(6) Uani 1 1 d . . . C14 C 0.7984(3) 0.6280(2) 0.6544(2) 0.0228(6) Uani 1 1 d . . . H14 H 0.7757 0.6417 0.7164 0.027 Uiso 1 1 calc R . . C15 C 0.8561(3) 0.6877(2) 0.5768(2) 0.0256(7) Uani 1 1 d . . . H15 H 0.8744 0.7413 0.5863 0.031 Uiso 1 1 calc R . . C16 C 0.8868(3) 0.6695(2) 0.4862(2) 0.0240(6) Uani 1 1 d . . . H16 H 0.9234 0.7123 0.4333 0.029 Uiso 1 1 calc R . . C17 C 0.8645(3) 0.5892(2) 0.4718(2) 0.0221(6) Uani 1 1 d . . . H17 H 0.8869 0.5768 0.4092 0.027 Uiso 1 1 calc R . . C18 C 0.7398(3) 0.0289(2) 0.4161(2) 0.0197(6) Uani 1 1 d . . . C19 C 0.8616(3) -0.0287(2) 0.3785(2) 0.0237(6) Uani 1 1 d . . . H19 H 0.8867 -0.0327 0.3132 0.028 Uiso 1 1 calc R . . C20 C 0.9461(3) -0.0801(2) 0.4370(2) 0.0271(7) Uani 1 1 d . . . H20 H 1.0287 -0.1199 0.4118 0.033 Uiso 1 1 calc R . . C21 C 0.9098(3) -0.0731(2) 0.5318(2) 0.0277(7) Uani 1 1 d . . . H21 H 0.9677 -0.1076 0.5716 0.033 Uiso 1 1 calc R . . C22 C 0.7890(3) -0.0159(3) 0.5689(2) 0.0296(7) Uani 1 1 d . . . H22 H 0.7650 -0.0116 0.6342 0.035 Uiso 1 1 calc R . . C23 C 0.7026(3) 0.0353(2) 0.5125(2) 0.0241(6) Uani 1 1 d . . . H23 H 0.6198 0.0740 0.5386 0.029 Uiso 1 1 calc R . . C24 C 0.5910(3) 0.0117(2) 0.3076(2) 0.0233(6) Uani 1 1 d . . . C25 C 0.6434(3) -0.0935(3) 0.3388(3) 0.0286(7) Uani 1 1 d . . . H25 H 0.7026 -0.1193 0.3772 0.034 Uiso 1 1 calc R . . C26 C 0.6084(4) -0.1610(3) 0.3132(3) 0.0379(9) Uani 1 1 d . . . H26 H 0.6441 -0.2328 0.3342 0.046 Uiso 1 1 calc R . . C27 C 0.5231(4) -0.1238(3) 0.2582(3) 0.0426(10) Uani 1 1 d . . . H27 H 0.5004 -0.1702 0.2408 0.051 Uiso 1 1 calc R . . C28 C 0.4689(4) -0.0184(3) 0.2272(3) 0.0399(9) Uani 1 1 d . . . H28 H 0.4094 0.0067 0.1891 0.048 Uiso 1 1 calc R . . C29 C 0.5023(3) 0.0496(3) 0.2524(3) 0.0310(7) Uani 1 1 d . . . H29 H 0.4651 0.1214 0.2322 0.037 Uiso 1 1 calc R . . C30 C 0.6448(3) 0.5331(2) 0.8417(2) 0.0214(6) Uani 1 1 d . . . C31 C 0.5262(3) 0.5965(3) 0.8771(2) 0.0271(7) Uani 1 1 d . . . H31 H 0.4605 0.6137 0.8467 0.033 Uiso 1 1 calc R . . C32 C 0.5047(3) 0.6344(3) 0.9571(3) 0.0341(8) Uani 1 1 d . . . H32 H 0.4236 0.6770 0.9818 0.041 Uiso 1 1 calc R . . C33 C 0.6002(4) 0.6104(3) 1.0010(3) 0.0342(8) Uani 1 1 d . . . H33 H 0.5847 0.6370 1.0554 0.041 Uiso 1 1 calc R . . C34 C 0.7184(4) 0.5478(3) 0.9661(3) 0.0341(8) Uani 1 1 d . . . H34 H 0.7841 0.5316 0.9962 0.041 Uiso 1 1 calc R . . C35 C 0.7405(3) 0.5089(3) 0.8867(2) 0.0288(7) Uani 1 1 d . . . H35 H 0.8214 0.4655 0.8629 0.035 Uiso 1 1 calc R . . C36 C 0.7639(3) 0.3472(2) 0.7643(2) 0.0192(6) Uani 1 1 d . . . C37 C 0.7042(3) 0.2756(2) 0.7861(2) 0.0264(7) Uani 1 1 d . . . H37 H 0.6184 0.2980 0.7860 0.032 Uiso 1 1 calc R . . C38 C 0.7697(3) 0.1714(3) 0.8080(2) 0.0300(7) Uani 1 1 d . . . H38 H 0.7289 0.1226 0.8225 0.036 Uiso 1 1 calc R . . C39 C 0.8946(3) 0.1388(2) 0.8087(2) 0.0281(7) Uani 1 1 d . . . H39 H 0.9391 0.0676 0.8241 0.034 Uiso 1 1 calc R . . C40 C 0.9554(3) 0.2098(3) 0.7869(2) 0.0258(7) Uani 1 1 d . . . H40 H 1.0410 0.1871 0.7875 0.031 Uiso 1 1 calc R . . C41 C 0.8902(3) 0.3141(2) 0.7642(2) 0.0231(6) Uani 1 1 d . . . H41 H 0.9315 0.3627 0.7487 0.028 Uiso 1 1 calc R . . Cl1 Cl 0.50096(5) 0.36200(4) 0.54071(4) 0.00999(12) Uani 1 1 d . . . Cu1 Cu 0.57881(3) 0.32287(3) 0.38357(3) 0.02088(10) Uani 1 1 d . . . Cu2 Cu 0.60438(3) 0.45985(3) 0.55672(3) 0.01918(9) Uani 1 1 d . . . H7 H 0.785(3) 0.189(3) 0.381(2) 0.018(8) Uiso 1 1 d . . . H8 H 0.745(3) 0.406(3) 0.296(3) 0.025(9) Uiso 1 1 d . . . H10 H 0.757(3) 0.491(3) 0.403(2) 0.017(8) Uiso 1 1 d . . . H11 H 0.813(4) 0.378(3) 0.576(3) 0.030(10) Uiso 1 1 d . . . O1 O 0.8273(2) 0.25214(16) 0.48578(16) 0.0244(5) Uani 1 1 d . . . P1 P 0.67766(7) 0.48331(6) 0.73766(5) 0.01758(15) Uani 1 1 d . . . P2 P 0.63622(7) 0.10122(6) 0.33633(5) 0.01822(15) Uani 1 1 d . . . S1 S 0.51923(7) 0.50148(5) 0.70419(5) 0.01828(15) Uani 1 1 d . . . S2 S 0.48703(7) 0.21080(6) 0.38833(6) 0.02148(16) Uani 1 1 d . . . F1 F 0.2646(2) 0.4040(2) 0.74491(16) 0.0486(6) Uani 1 1 d . . . F2 F 0.1445(3) 0.3036(2) 0.8011(2) 0.0634(8) Uani 1 1 d . . . F3 F 0.0562(2) 0.47475(19) 0.75940(16) 0.0434(5) Uani 1 1 d . . . F4 F 0.0264(2) 0.3937(2) 0.91470(18) 0.0526(7) Uani 1 1 d . . . F5 F 0.1462(3) 0.49595(18) 0.85756(17) 0.0481(6) Uani 1 1 d . . . F6 F 0.2350(2) 0.32419(18) 0.89961(17) 0.0455(6) Uani 1 1 d . . . P3 P 0.14563(8) 0.39924(7) 0.83039(6) 0.02656(18) Uani 1 1 d . . . C42 C 0.3871(9) -0.0243(7) -0.0020(9) 0.053(3) Uiso 0.3968(14) 1 d PD A 1 H42A H 0.3885 -0.0748 0.0584 0.079 Uiso 0.3968(14) 1 calc PR A 1 H42B H 0.4678 -0.0133 -0.0275 0.079 Uiso 0.3968(14) 1 calc PR A 1 H42C H 0.3706 -0.0496 -0.0479 0.079 Uiso 0.3968(14) 1 calc PR A 1 C43 C 0.2866(5) 0.0750(5) 0.0146(4) 0.0587(16) Uiso 0.3968(14) 1 d PD A 1 H43A H 0.3224 0.1305 -0.0203 0.070 Uiso 0.3968(14) 1 calc PR A 1 H43B H 0.2205 0.0845 -0.0163 0.070 Uiso 0.3968(14) 1 calc PR A 1 C44 C 0.1799(6) 0.1998(4) 0.1128(3) 0.0522(14) Uiso 0.794(3) 1 d PD A 1 H44A H 0.1140 0.2369 0.0763 0.063 Uiso 0.794(3) 1 calc PR A 1 H44B H 0.2481 0.2291 0.0827 0.063 Uiso 0.794(3) 1 calc PR A 1 C45 C 0.1274(4) 0.2137(4) 0.2152(3) 0.0435(11) Uiso 0.794(3) 1 d PD A 1 H45A H 0.0661 0.1782 0.2470 0.065 Uiso 0.794(3) 1 calc PR A 1 H45B H 0.0871 0.2869 0.2157 0.065 Uiso 0.794(3) 1 calc PR A 1 H45C H 0.1950 0.1849 0.2490 0.065 Uiso 0.794(3) 1 calc PR A 1 O2 O 0.2267(4) 0.0921(3) 0.1097(3) 0.0597(11) Uiso 0.3968(14) 1 d PD A 1 C42A C 0.1950(7) 0.0908(6) -0.0408(6) 0.0238(16) Uiso 0.3968(14) 1 d PD A 2 H42D H 0.1457 0.0452 -0.0067 0.036 Uiso 0.3968(14) 1 calc PR A 2 H42E H 0.2398 0.0753 -0.1040 0.036 Uiso 0.3968(14) 1 calc PR A 2 H42F H 0.1396 0.1622 -0.0481 0.036 Uiso 0.3968(14) 1 calc PR A 2 C43A C 0.2866(5) 0.0750(5) 0.0146(4) 0.0587(16) Uiso 0.3968(14) 1 d PD A 2 H43C H 0.3459 0.0041 0.0181 0.070 Uiso 0.3968(14) 1 calc PR A 2 H43D H 0.3345 0.1225 -0.0192 0.070 Uiso 0.3968(14) 1 calc PR A 2 O2A O 0.2267(4) 0.0921(3) 0.1097(3) 0.0597(11) Uiso 0.3968(14) 1 d P A 2 C46 C 0.1274(4) 0.2137(4) 0.2152(3) 0.0435(11) Uiso 0.072(3) 1 d PD B 3 Cl2 Cl 0.2632(10) 0.2339(13) 0.1444(10) 0.055(5) Uiso 0.072(3) 1 d PD B 3 Cl3 Cl 0.0731(16) 0.1181(10) 0.2216(13) 0.049(4) Uiso 0.072(3) 1 d PD B 3 C47 C 0.1861(16) 0.1046(15) 0.0687(9) 0.015(4) Uiso 0.134(3) 1 d PD C 4 H47A H 0.1995 0.1715 0.0392 0.018 Uiso 0.134(3) 1 calc PR C 4 H47B H 0.2703 0.0535 0.0690 0.018 Uiso 0.134(3) 1 calc PR C 4 Cl4 Cl 0.1210(14) 0.1101(10) 0.1875(8) 0.081(4) Uiso 0.134(3) 1 d PD C 4 Cl5 Cl 0.1402(12) 0.0813(9) -0.0170(8) 0.072(3) Uiso 0.134(3) 1 d PD C 4 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 C1 0.0206(14) 0.0193(14) 0.0200(14) -0.0061(11) -0.0029(11) -0.0053(11) C2 0.0305(17) 0.0261(16) 0.0239(16) -0.0110(13) -0.0051(13) -0.0091(13) C3 0.041(2) 0.0369(19) 0.0208(16) -0.0117(14) -0.0038(14) -0.0148(16) C4 0.040(2) 0.0343(18) 0.0204(16) -0.0050(13) -0.0004(14) -0.0174(16) C5 0.0330(17) 0.0251(16) 0.0233(16) -0.0062(12) -0.0028(13) -0.0138(14) C6 0.0215(14) 0.0192(14) 0.0194(14) -0.0090(11) -0.0030(11) -0.0042(11) C7 0.0150(13) 0.0208(14) 0.0196(14) -0.0063(11) -0.0013(11) -0.0056(11) C8 0.0185(14) 0.0196(14) 0.0196(14) -0.0065(11) -0.0023(11) -0.0072(11) C9 0.0156(13) 0.0192(14) 0.0215(14) -0.0086(11) -0.0023(11) -0.0036(11) C10 0.0160(13) 0.0182(13) 0.0192(14) -0.0049(11) -0.0038(11) -0.0046(11) C11 0.0135(13) 0.0193(14) 0.0189(14) -0.0051(11) -0.0026(11) -0.0041(11) C12 0.0154(13) 0.0176(13) 0.0212(14) -0.0050(11) -0.0069(11) -0.0032(11) C13 0.0177(13) 0.0172(13) 0.0204(14) -0.0036(11) -0.0069(11) -0.0043(11) C14 0.0257(15) 0.0227(15) 0.0242(15) -0.0087(12) -0.0076(12) -0.0078(12) C15 0.0269(16) 0.0212(15) 0.0330(17) -0.0070(13) -0.0070(13) -0.0113(13) C16 0.0206(15) 0.0207(15) 0.0290(16) -0.0030(12) -0.0038(12) -0.0082(12) C17 0.0215(15) 0.0250(15) 0.0204(14) -0.0051(12) -0.0035(12) -0.0089(12) C18 0.0202(14) 0.0157(13) 0.0232(15) -0.0052(11) -0.0043(11) -0.0057(11) C19 0.0243(15) 0.0178(14) 0.0260(16) -0.0065(12) -0.0033(12) -0.0044(12) C20 0.0225(15) 0.0200(15) 0.0360(18) -0.0061(13) -0.0064(13) -0.0042(12) C21 0.0289(17) 0.0214(15) 0.0328(18) -0.0001(13) -0.0127(14) -0.0079(13) C22 0.0333(18) 0.0317(17) 0.0246(16) -0.0043(13) -0.0071(14) -0.0124(15) C23 0.0226(15) 0.0251(15) 0.0224(15) -0.0057(12) -0.0027(12) -0.0067(12) C24 0.0225(15) 0.0219(15) 0.0271(16) -0.0117(12) -0.0008(12) -0.0078(12) C25 0.0280(17) 0.0243(16) 0.0338(18) -0.0097(14) 0.0005(14) -0.0121(13) C26 0.039(2) 0.0285(18) 0.050(2) -0.0186(17) 0.0023(17) -0.0168(16) C27 0.042(2) 0.044(2) 0.056(3) -0.029(2) 0.0015(19) -0.0240(18) C28 0.034(2) 0.050(2) 0.049(2) -0.0242(19) -0.0080(17) -0.0179(18) C29 0.0282(17) 0.0312(18) 0.0373(19) -0.0144(15) -0.0063(14) -0.0091(14) C30 0.0276(16) 0.0210(14) 0.0170(14) -0.0039(11) -0.0059(12) -0.0088(12) C31 0.0262(16) 0.0294(17) 0.0248(16) -0.0071(13) -0.0077(13) -0.0056(13) C32 0.0321(18) 0.0351(19) 0.0317(18) -0.0173(15) -0.0052(15) -0.0015(15) C33 0.043(2) 0.0367(19) 0.0260(17) -0.0154(15) -0.0092(15) -0.0091(16) C34 0.039(2) 0.039(2) 0.0296(18) -0.0135(15) -0.0150(15) -0.0083(16) C35 0.0281(17) 0.0314(17) 0.0278(17) -0.0123(14) -0.0096(13) -0.0038(14) C36 0.0237(14) 0.0173(13) 0.0147(13) -0.0021(10) -0.0063(11) -0.0044(11) C37 0.0273(16) 0.0231(15) 0.0284(16) -0.0051(13) -0.0075(13) -0.0072(13) C38 0.0383(19) 0.0202(15) 0.0302(17) -0.0020(13) -0.0067(15) -0.0116(14) C39 0.0339(18) 0.0200(15) 0.0205(15) -0.0033(12) -0.0041(13) -0.0012(13) C40 0.0243(15) 0.0282(16) 0.0201(15) -0.0081(12) -0.0063(12) -0.0004(13) C41 0.0259(16) 0.0245(15) 0.0192(14) -0.0068(12) -0.0048(12) -0.0072(13) Cl1 0.0087(3) 0.0109(3) 0.0121(3) -0.0064(2) -0.0017(2) -0.0026(2) Cu1 0.01934(19) 0.01886(18) 0.0256(2) -0.00999(15) -0.00314(15) -0.00499(14) Cu2 0.01758(18) 0.02180(19) 0.02020(19) -0.00784(14) -0.00429(14) -0.00597(14) O1 0.0276(11) 0.0187(10) 0.0265(11) -0.0062(9) -0.0119(9) -0.0016(9) P1 0.0192(4) 0.0176(3) 0.0172(3) -0.0040(3) -0.0058(3) -0.0057(3) P2 0.0189(4) 0.0158(3) 0.0202(4) -0.0063(3) -0.0032(3) -0.0050(3) S1 0.0184(3) 0.0193(3) 0.0178(3) -0.0046(3) -0.0052(3) -0.0056(3) S2 0.0184(3) 0.0185(3) 0.0280(4) -0.0099(3) -0.0034(3) -0.0041(3) F1 0.0360(12) 0.0579(15) 0.0357(12) -0.0001(11) -0.0038(10) -0.0100(11) F2 0.0620(17) 0.0448(15) 0.108(2) -0.0361(15) -0.0345(17) -0.0152(13) F3 0.0385(12) 0.0519(14) 0.0378(12) -0.0090(10) -0.0176(10) -0.0061(11) F4 0.0404(13) 0.0494(14) 0.0492(15) 0.0039(11) 0.0039(11) -0.0173(11) F5 0.0822(18) 0.0354(12) 0.0437(13) -0.0071(10) -0.0235(13) -0.0302(12) F6 0.0491(14) 0.0438(13) 0.0444(13) 0.0153(10) -0.0257(11) -0.0228(11) P3 0.0305(4) 0.0265(4) 0.0280(4) -0.0047(3) -0.0093(3) -0.0135(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 C1 C2 1.394(4) . ? C1 C6 1.415(4) . ? C1 P2 1.818(3) . ? C2 C3 1.387(5) . ? C2 H2 0.9500 . ? C3 C4 1.385(5) . ? C3 H3 0.9500 . ? C4 C5 1.388(5) . ? C4 H4 0.9500 . ? C5 C6 1.401(4) . ? C5 H5 0.9500 . ? C6 C7 1.479(4) . ? C7 C8 1.373(4) . ? C7 Cu1 2.112(3) . ? C7 H7 1.03(3) . ? C8 C9 1.494(4) . ? C8 Cu1 2.164(3) . ? C8 H8 0.97(4) . ? C9 O1 1.224(4) . ? C9 C10 1.489(4) . ? C10 C11 1.373(4) . ? C10 Cu2 2.108(3) . ? C10 H10 0.92(3) . ? C11 C12 1.481(4) . ? C11 Cu2 2.089(3) . ? C11 H11 0.89(4) . ? C12 C17 1.401(4) . ? C12 C13 1.412(4) . ? C13 C14 1.399(4) . ? C13 P1 1.812(3) . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C15 C16 1.382(5) . ? C15 H15 0.9500 . ? C16 C17 1.389(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.398(4) . ? C18 C23 1.402(4) . ? C18 P2 1.803(3) . ? C19 C20 1.392(5) . ? C19 H19 0.9500 . ? C20 C21 1.381(5) . ? C20 H20 0.9500 . ? C21 C22 1.386(5) . ? C21 H21 0.9500 . ? C22 C23 1.387(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.392(5) . ? C24 C29 1.400(5) . ? C24 P2 1.800(3) . ? C25 C26 1.399(5) . ? C25 H25 0.9500 . ? C26 C27 1.366(6) . ? C26 H26 0.9500 . ? C27 C28 1.397(6) . ? C27 H27 0.9500 . ? C28 C29 1.389(5) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.392(4) . ? C30 C35 1.394(4) . ? C30 P1 1.799(3) . ? C31 C32 1.392(5) . ? C31 H31 0.9500 . ? C32 C33 1.382(5) . ? C32 H32 0.9500 . ? C33 C34 1.384(5) . ? C33 H33 0.9500 . ? C34 C35 1.389(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.393(4) . ? C36 C41 1.397(4) . ? C36 P1 1.816(3) . ? C37 C38 1.392(5) . ? C37 H37 0.9500 . ? C38 C39 1.385(5) . ? C38 H38 0.9500 . ? C39 C40 1.394(5) . ? C39 H39 0.9500 . ? C40 C41 1.393(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? Cl1 Cu2 2.3330(7) . ? Cl1 Cu1 2.4155(7) . ? Cl1 Cu2 2.5906(7) 2_666 ? Cu1 S2 2.2767(8) . ? Cu1 S1 2.4872(8) 2_666 ? Cu2 S1 2.2948(8) . ? Cu2 Cl1 2.5907(7) 2_666 ? P1 S1 2.0221(10) . ? P2 S2 1.9936(10) . ? S1 Cu1 2.4872(8) 2_666 ? F1 P3 1.599(2) . ? F2 P3 1.592(2) . ? F3 P3 1.608(2) . ? F4 P3 1.594(2) . ? F5 P3 1.586(2) . ? F6 P3 1.588(2) . ? C42 C43 1.501(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 O2 1.435(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O2 1.449(4) . ? C44 C45 1.517(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C47 Cl5 1.727(5) . ? C47 Cl4 1.728(5) . ? C47 H47A 0.9900 . ? C47 H47B 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 C2 C1 C6 120.0(3) . . ? C2 C1 P2 121.2(2) . . ? C6 C1 P2 118.5(2) . . ? C3 C2 C1 120.1(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.5(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 118.6(3) . . ? C5 C6 C7 120.6(3) . . ? C1 C6 C7 120.6(3) . . ? C8 C7 C6 126.8(3) . . ? C8 C7 Cu1 73.36(17) . . ? C6 C7 Cu1 107.9(2) . . ? C8 C7 H7 111.9(19) . . ? C6 C7 H7 120.3(19) . . ? Cu1 C7 H7 97.1(19) . . ? C7 C8 C9 117.6(3) . . ? C7 C8 Cu1 69.20(17) . . ? C9 C8 Cu1 104.62(19) . . ? C7 C8 H8 125(2) . . ? C9 C8 H8 117(2) . . ? Cu1 C8 H8 100(2) . . ? O1 C9 C10 121.9(3) . . ? O1 C9 C8 122.2(3) . . ? C10 C9 C8 116.0(3) . . ? C11 C10 C9 120.4(3) . . ? C11 C10 Cu2 70.17(17) . . ? C9 C10 Cu2 103.64(19) . . ? C11 C10 H10 121(2) . . ? C9 C10 H10 118(2) . . ? Cu2 C10 H10 104(2) . . ? C10 C11 C12 124.2(3) . . ? C10 C11 Cu2 71.65(17) . . ? C12 C11 Cu2 109.58(19) . . ? C10 C11 H11 118(3) . . ? C12 C11 H11 117(3) . . ? Cu2 C11 H11 98(3) . . ? C17 C12 C13 118.7(3) . . ? C17 C12 C11 119.9(3) . . ? C13 C12 C11 121.3(3) . . ? C14 C13 C12 120.2(3) . . ? C14 C13 P1 119.4(2) . . ? C12 C13 P1 119.9(2) . . ? C15 C14 C13 119.7(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.4(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 120.5(3) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C19 C18 C23 120.2(3) . . ? C19 C18 P2 118.5(2) . . ? C23 C18 P2 121.1(2) . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 121.2(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.7(3) . . ? C22 C23 H23 120.7 . . ? C18 C23 H23 120.7 . . ? C25 C24 C29 120.0(3) . . ? C25 C24 P2 121.1(3) . . ? C29 C24 P2 118.9(2) . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.8(3) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 119.7(4) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C24 119.7(3) . . ? C28 C29 H29 120.2 . . ? C24 C29 H29 120.2 . . ? C31 C30 C35 119.6(3) . . ? C31 C30 P1 121.2(2) . . ? C35 C30 P1 119.2(2) . . ? C32 C31 C30 119.6(3) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C33 C32 C31 120.5(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 120.3(3) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C35 119.6(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C30 120.5(3) . . ? C34 C35 H35 119.7 . . ? C30 C35 H35 119.7 . . ? C37 C36 C41 119.8(3) . . ? C37 C36 P1 120.1(2) . . ? C41 C36 P1 120.1(2) . . ? C38 C37 C36 120.2(3) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C39 C38 C37 119.9(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 120.4(3) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 119.8(3) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C36 119.9(3) . . ? C40 C41 H41 120.1 . . ? C36 C41 H41 120.1 . . ? Cu2 Cl1 Cu1 110.15(3) . . ? Cu2 Cl1 Cu2 78.76(2) . 2_666 ? Cu1 Cl1 Cu2 81.11(2) . 2_666 ? C7 Cu1 C8 37.44(11) . . ? C7 Cu1 S2 102.24(8) . . ? C8 Cu1 S2 139.68(8) . . ? C7 Cu1 Cl1 125.06(8) . . ? C8 Cu1 Cl1 102.56(8) . . ? S2 Cu1 Cl1 104.95(3) . . ? C7 Cu1 S1 115.78(8) . 2_666 ? C8 Cu1 S1 93.14(8) . 2_666 ? S2 Cu1 S1 112.26(3) . 2_666 ? Cl1 Cu1 S1 96.37(2) . 2_666 ? C11 Cu2 C10 38.18(11) . . ? C11 Cu2 S1 104.35(8) . . ? C10 Cu2 S1 142.06(8) . . ? C11 Cu2 Cl1 131.65(8) . . ? C10 Cu2 Cl1 105.27(8) . . ? S1 Cu2 Cl1 108.39(3) . . ? C11 Cu2 Cl1 109.27(9) . 2_666 ? C10 Cu2 Cl1 93.48(8) . 2_666 ? S1 Cu2 Cl1 96.65(3) . 2_666 ? Cl1 Cu2 Cl1 101.24(2) . 2_666 ? C30 P1 C13 107.94(14) . . ? C30 P1 C36 107.83(14) . . ? C13 P1 C36 109.35(14) . . ? C30 P1 S1 111.36(11) . . ? C13 P1 S1 111.74(10) . . ? C36 P1 S1 108.54(10) . . ? C24 P2 C18 107.52(14) . . ? C24 P2 C1 107.51(14) . . ? C18 P2 C1 105.84(14) . . ? C24 P2 S2 110.83(11) . . ? C18 P2 S2 114.01(10) . . ? C1 P2 S2 110.79(10) . . ? P1 S1 Cu2 98.61(4) . . ? P1 S1 Cu1 113.77(4) . 2_666 ? Cu2 S1 Cu1 85.78(3) . 2_666 ? P2 S2 Cu1 99.91(4) . . ? F5 P3 F6 90.88(13) . . ? F5 P3 F2 178.83(16) . . ? F6 P3 F2 90.17(15) . . ? F5 P3 F4 90.92(15) . . ? F6 P3 F4 90.66(14) . . ? F2 P3 F4 89.58(16) . . ? F5 P3 F1 89.82(15) . . ? F6 P3 F1 89.76(13) . . ? F2 P3 F1 89.66(16) . . ? F4 P3 F1 179.14(16) . . ? F5 P3 F3 89.42(13) . . ? F6 P3 F3 179.41(16) . . ? F2 P3 F3 89.53(14) . . ? F4 P3 F3 89.84(14) . . ? F1 P3 F3 89.73(13) . . ? O2 C43 C42 120.8(6) . . ? O2 C43 H43A 107.1 . . ? C42 C43 H43A 107.1 . . ? O2 C43 H43B 107.1 . . ? C42 C43 H43B 107.1 . . ? H43A C43 H43B 106.8 . . ? O2 C44 C45 110.6(4) . . ? O2 C44 H44A 109.5 . . ? C45 C44 H44A 109.5 . . ? O2 C44 H44B 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? C43 O2 C44 112.3(4) . . ? H42D C42A H42E 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? Cl5 C47 Cl4 133.4(11) . . ? Cl5 C47 H47A 103.9 . . ? Cl4 C47 H47A 103.9 . . ? Cl5 C47 H47B 103.9 . . ? Cl4 C47 H47B 103.9 . . ? H47A C47 H47B 105.4 . . ? 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 -0.3(5) . . . . ? P2 C1 C2 C3 174.0(3) . . . . ? C1 C2 C3 C4 -2.2(5) . . . . ? C2 C3 C4 C5 2.9(6) . . . . ? C3 C4 C5 C6 -1.0(5) . . . . ? C4 C5 C6 C1 -1.5(5) . . . . ? C4 C5 C6 C7 173.5(3) . . . . ? C2 C1 C6 C5 2.1(5) . . . . ? P2 C1 C6 C5 -172.3(2) . . . . ? C2 C1 C6 C7 -172.9(3) . . . . ? P2 C1 C6 C7 12.7(4) . . . . ? C5 C6 C7 C8 31.3(5) . . . . ? C1 C6 C7 C8 -153.8(3) . . . . ? C5 C6 C7 Cu1 113.5(3) . . . . ? C1 C6 C7 Cu1 -71.6(3) . . . . ? C6 C7 C8 C9 -163.8(3) . . . . ? Cu1 C7 C8 C9 96.1(2) . . . . ? C6 C7 C8 Cu1 100.1(3) . . . . ? C7 C8 C9 O1 5.5(4) . . . . ? Cu1 C8 C9 O1 79.4(3) . . . . ? C7 C8 C9 C10 -174.8(3) . . . . ? Cu1 C8 C9 C10 -100.9(2) . . . . ? O1 C9 C10 C11 -1.3(4) . . . . ? C8 C9 C10 C11 179.0(3) . . . . ? O1 C9 C10 Cu2 -76.1(3) . . . . ? C8 C9 C10 Cu2 104.2(2) . . . . ? C9 C10 C11 C12 163.8(3) . . . . ? Cu2 C10 C11 C12 -101.6(3) . . . . ? C9 C10 C11 Cu2 -94.5(3) . . . . ? C10 C11 C12 C17 -33.0(4) . . . . ? Cu2 C11 C12 C17 -113.7(3) . . . . ? C10 C11 C12 C13 149.6(3) . . . . ? Cu2 C11 C12 C13 69.0(3) . . . . ? C17 C12 C13 C14 -2.4(4) . . . . ? C11 C12 C13 C14 175.0(3) . . . . ? C17 C12 C13 P1 169.0(2) . . . . ? C11 C12 C13 P1 -13.7(4) . . . . ? C12 C13 C14 C15 1.0(4) . . . . ? P1 C13 C14 C15 -170.4(2) . . . . ? C13 C14 C15 C16 1.4(5) . . . . ? C14 C15 C16 C17 -2.3(5) . . . . ? C15 C16 C17 C12 0.8(5) . . . . ? C13 C12 C17 C16 1.5(4) . . . . ? C11 C12 C17 C16 -175.9(3) . . . . ? C23 C18 C19 C20 0.2(5) . . . . ? P2 C18 C19 C20 175.9(2) . . . . ? C18 C19 C20 C21 -0.8(5) . . . . ? C19 C20 C21 C22 0.7(5) . . . . ? C20 C21 C22 C23 0.0(5) . . . . ? C21 C22 C23 C18 -0.5(5) . . . . ? C19 C18 C23 C22 0.4(4) . . . . ? P2 C18 C23 C22 -175.2(2) . . . . ? C29 C24 C25 C26 1.1(5) . . . . ? P2 C24 C25 C26 -178.4(3) . . . . ? C24 C25 C26 C27 -0.2(5) . . . . ? C25 C26 C27 C28 -0.5(6) . . . . ? C26 C27 C28 C29 0.2(6) . . . . ? C27 C28 C29 C24 0.7(6) . . . . ? C25 C24 C29 C28 -1.3(5) . . . . ? P2 C24 C29 C28 178.2(3) . . . . ? C35 C30 C31 C32 -0.4(5) . . . . ? P1 C30 C31 C32 -179.3(3) . . . . ? C30 C31 C32 C33 0.7(6) . . . . ? C31 C32 C33 C34 -0.4(6) . . . . ? C32 C33 C34 C35 -0.2(6) . . . . ? C33 C34 C35 C30 0.5(6) . . . . ? C31 C30 C35 C34 -0.2(5) . . . . ? P1 C30 C35 C34 178.8(3) . . . . ? C41 C36 C37 C38 0.3(5) . . . . ? P1 C36 C37 C38 -179.0(3) . . . . ? C36 C37 C38 C39 0.3(5) . . . . ? C37 C38 C39 C40 -0.4(5) . . . . ? C38 C39 C40 C41 -0.1(5) . . . . ? C39 C40 C41 C36 0.6(5) . . . . ? C37 C36 C41 C40 -0.7(4) . . . . ? P1 C36 C41 C40 178.5(2) . . . . ? C6 C7 Cu1 C8 -124.1(3) . . . . ? C8 C7 Cu1 S2 -179.68(16) . . . . ? C6 C7 Cu1 S2 56.2(2) . . . . ? C8 C7 Cu1 Cl1 -61.3(2) . . . . ? C6 C7 Cu1 Cl1 174.53(15) . . . . ? C8 C7 Cu1 S1 57.96(19) . . . 2_666 ? C6 C7 Cu1 S1 -66.2(2) . . . 2_666 ? C9 C8 Cu1 C7 -114.4(3) . . . . ? C7 C8 Cu1 S2 0.5(2) . . . . ? C9 C8 Cu1 S2 -113.91(18) . . . . ? C7 C8 Cu1 Cl1 132.61(17) . . . . ? C9 C8 Cu1 Cl1 18.22(19) . . . . ? C7 C8 Cu1 S1 -130.14(17) . . . 2_666 ? C9 C8 Cu1 S1 115.47(18) . . . 2_666 ? Cu2 Cl1 Cu1 C7 55.56(10) . . . . ? Cu2 Cl1 Cu1 C7 130.04(10) 2_666 . . . ? Cu2 Cl1 Cu1 C8 22.43(9) . . . . ? Cu2 Cl1 Cu1 C8 96.91(8) 2_666 . . . ? Cu2 Cl1 Cu1 S2 172.65(3) . . . . ? Cu2 Cl1 Cu1 S2 -112.87(3) 2_666 . . . ? Cu2 Cl1 Cu1 S1 -72.24(3) . . . 2_666 ? Cu2 Cl1 Cu1 S1 2.24(2) 2_666 . . 2_666 ? C12 C11 Cu2 C10 120.7(3) . . . . ? C10 C11 Cu2 S1 -172.56(16) . . . . ? C12 C11 Cu2 S1 -51.9(2) . . . . ? C10 C11 Cu2 Cl1 55.9(2) . . . . ? C12 C11 Cu2 Cl1 176.54(15) . . . . ? C10 C11 Cu2 Cl1 -70.08(17) . . . 2_666 ? C12 C11 Cu2 Cl1 50.6(2) . . . 2_666 ? C9 C10 Cu2 C11 117.8(3) . . . . ? C11 C10 Cu2 S1 11.8(2) . . . . ? C9 C10 Cu2 S1 129.57(16) . . . . ? C11 C10 Cu2 Cl1 -140.11(16) . . . . ? C9 C10 Cu2 Cl1 -22.3(2) . . . . ? C11 C10 Cu2 Cl1 117.24(17) . . . 2_666 ? C9 C10 Cu2 Cl1 -124.97(18) . . . 2_666 ? Cu1 Cl1 Cu2 C11 -52.76(12) . . . . ? Cu2 Cl1 Cu2 C11 -128.83(11) 2_666 . . . ? Cu1 Cl1 Cu2 C10 -20.73(9) . . . . ? Cu2 Cl1 Cu2 C10 -96.79(9) 2_666 . . . ? Cu1 Cl1 Cu2 S1 177.05(3) . . . . ? Cu2 Cl1 Cu2 S1 100.98(3) 2_666 . . . ? Cu1 Cl1 Cu2 Cl1 76.07(3) . . . 2_666 ? Cu2 Cl1 Cu2 Cl1 0.0 2_666 . . 2_666 ? C31 C30 P1 C13 109.0(3) . . . . ? C35 C30 P1 C13 -70.0(3) . . . . ? C31 C30 P1 C36 -133.0(3) . . . . ? C35 C30 P1 C36 48.0(3) . . . . ? C31 C30 P1 S1 -14.0(3) . . . . ? C35 C30 P1 S1 167.0(2) . . . . ? C14 C13 P1 C30 -5.8(3) . . . . ? C12 C13 P1 C30 -177.2(2) . . . . ? C14 C13 P1 C36 -122.9(2) . . . . ? C12 C13 P1 C36 65.7(3) . . . . ? C14 C13 P1 S1 117.0(2) . . . . ? C12 C13 P1 S1 -54.5(2) . . . . ? C37 C36 P1 C30 102.6(3) . . . . ? C41 C36 P1 C30 -76.7(3) . . . . ? C37 C36 P1 C13 -140.3(2) . . . . ? C41 C36 P1 C13 40.5(3) . . . . ? C37 C36 P1 S1 -18.2(3) . . . . ? C41 C36 P1 S1 162.6(2) . . . . ? C25 C24 P2 C18 -5.6(3) . . . . ? C29 C24 P2 C18 174.9(3) . . . . ? C25 C24 P2 C1 108.0(3) . . . . ? C29 C24 P2 C1 -71.5(3) . . . . ? C25 C24 P2 S2 -130.8(3) . . . . ? C29 C24 P2 S2 49.7(3) . . . . ? C19 C18 P2 C24 74.5(3) . . . . ? C23 C18 P2 C24 -109.8(3) . . . . ? C19 C18 P2 C1 -40.2(3) . . . . ? C23 C18 P2 C1 135.5(2) . . . . ? C19 C18 P2 S2 -162.2(2) . . . . ? C23 C18 P2 S2 13.4(3) . . . . ? C2 C1 P2 C24 3.8(3) . . . . ? C6 C1 P2 C24 178.2(2) . . . . ? C2 C1 P2 C18 118.5(3) . . . . ? C6 C1 P2 C18 -67.1(3) . . . . ? C2 C1 P2 S2 -117.4(2) . . . . ? C6 C1 P2 S2 56.9(3) . . . . ? C30 P1 S1 Cu2 169.12(11) . . . . ? C13 P1 S1 Cu2 48.32(11) . . . . ? C36 P1 S1 Cu2 -72.33(10) . . . . ? C30 P1 S1 Cu1 79.96(11) . . . 2_666 ? C13 P1 S1 Cu1 -40.84(11) . . . 2_666 ? C36 P1 S1 Cu1 -161.49(10) . . . 2_666 ? C11 Cu2 S1 P1 -3.89(9) . . . . ? C10 Cu2 S1 P1 -11.37(14) . . . . ? Cl1 Cu2 S1 P1 140.01(3) . . . . ? Cl1 Cu2 S1 P1 -115.77(3) 2_666 . . . ? C11 Cu2 S1 Cu1 109.54(9) . . . 2_666 ? C10 Cu2 S1 Cu1 102.06(14) . . . 2_666 ? Cl1 Cu2 S1 Cu1 -106.56(3) . . . 2_666 ? Cl1 Cu2 S1 Cu1 -2.34(2) 2_666 . . 2_666 ? C24 P2 S2 Cu1 -168.08(12) . . . . ? C18 P2 S2 Cu1 70.45(11) . . . . ? C1 P2 S2 Cu1 -48.81(11) . . . . ? C7 Cu1 S2 P2 1.71(9) . . . . ? C8 Cu1 S2 P2 1.41(14) . . . . ? Cl1 Cu1 S2 P2 -130.07(4) . . . . ? S1 Cu1 S2 P2 126.43(4) 2_666 . . . ? C42 C43 O2 C44 152.7(7) . . . . ? C45 C44 O2 C43 -175.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.201 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.102 # Attachment '- ijf0829a.cif' data_ijf0829a _database_code_depnum_ccdc_archive 'CCDC 801874' #TrackingRef '- ijf0829a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H64 Cu2 O4 P4 S4, 2(F6 P)' _chemical_formula_sum 'C82 H64 Cu2 F12 O4 P6 S4' _chemical_formula_weight 1782.47 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 _symmetry_space_group_name_Hall '-P 2ybc' 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 25.838(3) _cell_length_b 25.365(3) _cell_length_c 14.7220(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.563(2) _cell_angle_gamma 90.00 _cell_volume 9564.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8515 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.10 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.684 _exptl_absorpt_correction_T_max 0.9528 _exptl_absorpt_process_details 'SADABS v2.10; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _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_% ? _diffrn_reflns_number 16818 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1269 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 0.79 _diffrn_reflns_theta_max 25.10 _reflns_number_total 16818 _reflns_number_gt 8592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The crystals contained disordered solvent (a mixture of CH2Cl2 and Et2O) which could not be modelled as discrete atoms. Therefore the SQUEEZE algorithm was used to account for the solvent (see below). It is assumed that the oxygen ligands bound to the copper are from water molecules but suitable locations for the hydrogens could not be obtained by either difference map or using a riding model. ; _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^)+(0.0874P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16818 _refine_ls_number_parameters 992 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1422 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.2117 _refine_ls_wR_factor_gt 0.1993 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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 C1 C 0.4406(2) 0.6117(2) 0.4581(4) 0.0276(15) Uani 1 1 d . . . C2 C 0.4367(2) 0.6409(2) 0.3784(5) 0.0350(17) Uani 1 1 d . . . H2 H 0.4050 0.6583 0.3564 0.042 Uiso 1 1 calc R . . C3 C 0.4792(2) 0.6447(2) 0.3307(5) 0.0378(17) Uani 1 1 d . . . H3 H 0.4767 0.6652 0.2763 0.045 Uiso 1 1 calc R . . C4 C 0.5252(2) 0.6190(2) 0.3615(4) 0.0362(16) Uani 1 1 d . . . H4 H 0.5544 0.6218 0.3287 0.043 Uiso 1 1 calc R . . C5 C 0.5285(2) 0.5891(2) 0.4404(4) 0.0346(16) Uani 1 1 d . . . H5 H 0.5599 0.5708 0.4612 0.042 Uiso 1 1 calc R . . C6 C 0.4870(2) 0.5855(2) 0.4892(4) 0.0278(15) Uani 1 1 d . . . H6 H 0.4898 0.5653 0.5439 0.033 Uiso 1 1 calc R . . C7 C 0.3983(2) 0.5668(2) 0.6168(5) 0.0316(16) Uani 1 1 d . . . C8 C 0.4363(2) 0.5758(3) 0.6951(5) 0.0388(18) Uani 1 1 d . . . H8 H 0.4559 0.6075 0.7007 0.047 Uiso 1 1 calc R . . C9 C 0.4440(3) 0.5378(3) 0.7626(5) 0.0434(18) Uani 1 1 d . . . H9 H 0.4696 0.5433 0.8143 0.052 Uiso 1 1 calc R . . C10 C 0.4157(3) 0.4924(3) 0.7563(5) 0.0417(18) Uani 1 1 d . . . H10 H 0.4212 0.4671 0.8042 0.050 Uiso 1 1 calc R . . C11 C 0.3780(3) 0.4823(3) 0.6793(6) 0.047(2) Uani 1 1 d . . . H11 H 0.3591 0.4500 0.6745 0.057 Uiso 1 1 calc R . . C12 C 0.3689(2) 0.5203(2) 0.6106(5) 0.0390(17) Uani 1 1 d . . . H12 H 0.3429 0.5146 0.5596 0.047 Uiso 1 1 calc R . . C13 C 0.3928(2) 0.6804(2) 0.5802(4) 0.0301(15) Uani 1 1 d . . . C14 C 0.4312(2) 0.7154(2) 0.5605(5) 0.0362(17) Uani 1 1 d . . . H14 H 0.4575 0.7033 0.5260 0.043 Uiso 1 1 calc R . . C15 C 0.4322(2) 0.7669(2) 0.5897(5) 0.0370(17) Uani 1 1 d . . . H15 H 0.4586 0.7904 0.5753 0.044 Uiso 1 1 calc R . . C16 C 0.3941(3) 0.7839(2) 0.6402(5) 0.0450(19) Uani 1 1 d . . . H16 H 0.3938 0.8196 0.6596 0.054 Uiso 1 1 calc R . . C17 C 0.3558(2) 0.7492(2) 0.6633(5) 0.048(2) Uani 1 1 d . . . H17 H 0.3306 0.7614 0.6999 0.058 Uiso 1 1 calc R . . C18 C 0.3541(2) 0.6970(2) 0.6335(5) 0.0404(18) Uani 1 1 d . . . C19 C 0.3139(2) 0.6616(2) 0.6590(5) 0.0413(18) Uani 1 1 d . . . H19 H 0.3208 0.6248 0.6583 0.050 Uiso 1 1 calc R . . C20 C 0.2679(3) 0.6769(3) 0.6836(5) 0.048(2) Uani 1 1 d . . . H20 H 0.2592 0.7133 0.6780 0.057 Uiso 1 1 calc R . . C21 C 0.2294(3) 0.6411(3) 0.7190(5) 0.0471(19) Uani 1 1 d . . . C22 C 0.2396(2) 0.5832(2) 0.7253(5) 0.0396(17) Uani 1 1 d . . . H22 H 0.2757 0.5708 0.7188 0.047 Uiso 1 1 calc R . . C23 C 0.2106(2) 0.5529(3) 0.7757(5) 0.0432(19) Uani 1 1 d . . . H23 H 0.1897 0.5734 0.8160 0.052 Uiso 1 1 calc R . . C24 C 0.2251(2) 0.4988(3) 0.8100(4) 0.0393(17) Uani 1 1 d . . . C25 C 0.2782(3) 0.4874(3) 0.8404(5) 0.056(2) Uani 1 1 d . . . H25 H 0.3041 0.5135 0.8366 0.068 Uiso 1 1 calc R . . C26 C 0.2924(3) 0.4376(3) 0.8759(5) 0.061(2) Uani 1 1 d . . . H26 H 0.3280 0.4300 0.8966 0.073 Uiso 1 1 calc R . . C27 C 0.2549(3) 0.3997(4) 0.8810(5) 0.062(2) Uani 1 1 d . . . H27 H 0.2650 0.3659 0.9053 0.074 Uiso 1 1 calc R . . C28 C 0.2036(3) 0.4096(4) 0.8518(5) 0.065(2) Uani 1 1 d . . . H28 H 0.1783 0.3827 0.8550 0.078 Uiso 1 1 calc R . . C29 C 0.1882(2) 0.4597(3) 0.8168(4) 0.0445(19) Uani 1 1 d . . . C30 C 0.0850(2) 0.4113(3) 0.7831(6) 0.051(2) Uani 1 1 d . . . C31 C 0.0776(3) 0.3785(3) 0.7083(6) 0.057(2) Uani 1 1 d . . . H31 H 0.0889 0.3889 0.6521 0.069 Uiso 1 1 calc R . . C32 C 0.0534(3) 0.3296(3) 0.7153(8) 0.076(3) Uani 1 1 d . . . H32 H 0.0494 0.3066 0.6640 0.092 Uiso 1 1 calc R . . C33 C 0.0357(4) 0.3147(4) 0.7925(9) 0.090(4) Uani 1 1 d . . . H33 H 0.0177 0.2821 0.7945 0.108 Uiso 1 1 calc R . . C34 C 0.0433(3) 0.3465(4) 0.8698(8) 0.088(4) Uani 1 1 d . . . H34 H 0.0323 0.3345 0.9253 0.105 Uiso 1 1 calc R . . C35 C 0.0676(3) 0.3973(4) 0.8673(7) 0.079(3) Uani 1 1 d . . . H35 H 0.0718 0.4202 0.9189 0.095 Uiso 1 1 calc R . . C36 C 0.0998(3) 0.5189(3) 0.8580(5) 0.057(2) Uani 1 1 d . . . C37 C 0.0586(3) 0.5542(3) 0.8305(6) 0.061(2) Uani 1 1 d . . . H37 H 0.0417 0.5544 0.7691 0.073 Uiso 1 1 calc R . . C38 C 0.0435(3) 0.5885(4) 0.8954(7) 0.075(3) Uani 1 1 d . . . H38 H 0.0146 0.6111 0.8778 0.090 Uiso 1 1 calc R . . C39 C 0.0677(4) 0.5915(4) 0.9823(7) 0.098(4) Uani 1 1 d . . . H39 H 0.0572 0.6164 1.0244 0.118 Uiso 1 1 calc R . . C40 C 0.1080(4) 0.5570(4) 1.0074(6) 0.107(4) Uani 1 1 d . . . H40 H 0.1247 0.5577 1.0688 0.129 Uiso 1 1 calc R . . C41 C 0.1248(3) 0.5222(4) 0.9484(5) 0.084(3) Uani 1 1 d . . . H41 H 0.1536 0.4998 0.9681 0.101 Uiso 1 1 calc R . . C42 C 0.4178(2) 0.3996(2) 0.2364(4) 0.0302(15) Uani 1 1 d . . . C43 C 0.4225(2) 0.3680(2) 0.3139(5) 0.0346(16) Uani 1 1 d . . . H43 H 0.4079 0.3793 0.3665 0.042 Uiso 1 1 calc R . . C44 C 0.4484(3) 0.3199(2) 0.3156(6) 0.0466(19) Uani 1 1 d . . . H44 H 0.4507 0.2981 0.3684 0.056 Uiso 1 1 calc R . . C45 C 0.4707(3) 0.3042(3) 0.2407(7) 0.056(2) Uani 1 1 d . . . H45 H 0.4884 0.2714 0.2423 0.067 Uiso 1 1 calc R . . C46 C 0.4680(3) 0.3340(3) 0.1651(7) 0.073(3) Uani 1 1 d . . . H46 H 0.4845 0.3226 0.1145 0.087 Uiso 1 1 calc R . . C47 C 0.4406(2) 0.3822(3) 0.1606(5) 0.0405(18) Uani 1 1 d . . . H47 H 0.4377 0.4029 0.1064 0.049 Uiso 1 1 calc R . . C48 C 0.4062(2) 0.5030(2) 0.1531(4) 0.0272(14) Uani 1 1 d . . . C49 C 0.4448(2) 0.5391(2) 0.1818(4) 0.0303(15) Uani 1 1 d . . . H49 H 0.4575 0.5419 0.2452 0.036 Uiso 1 1 calc R . . C50 C 0.4653(2) 0.5717(3) 0.1191(5) 0.0420(18) Uani 1 1 d . . . H50 H 0.4918 0.5964 0.1397 0.050 Uiso 1 1 calc R . . C51 C 0.4473(3) 0.5678(3) 0.0292(5) 0.056(2) Uani 1 1 d . . . H51 H 0.4623 0.5888 -0.0138 0.067 Uiso 1 1 calc R . . C52 C 0.4072(3) 0.5335(4) -0.0011(5) 0.085(3) Uani 1 1 d . . . H52 H 0.3936 0.5325 -0.0643 0.102 Uiso 1 1 calc R . . C53 C 0.3866(3) 0.5007(3) 0.0598(5) 0.056(2) Uani 1 1 d . . . H53 H 0.3594 0.4767 0.0386 0.067 Uiso 1 1 calc R . . C54 C 0.3151(2) 0.4441(2) 0.1872(4) 0.0262(14) Uani 1 1 d . . . C55 C 0.3012(2) 0.3927(3) 0.1573(4) 0.0385(17) Uani 1 1 d . . . H55 H 0.3271 0.3660 0.1604 0.046 Uiso 1 1 calc R . . C56 C 0.2503(2) 0.3809(3) 0.1235(5) 0.0469(19) Uani 1 1 d . . . H56 H 0.2414 0.3461 0.1036 0.056 Uiso 1 1 calc R . . C57 C 0.2118(2) 0.4197(3) 0.1182(4) 0.0396(17) Uani 1 1 d . . . H57 H 0.1766 0.4116 0.0949 0.047 Uiso 1 1 calc R . . C58 C 0.2256(2) 0.4697(3) 0.1475(4) 0.0361(16) Uani 1 1 d . . . H58 H 0.1994 0.4962 0.1441 0.043 Uiso 1 1 calc R . . C59 C 0.2761(2) 0.4830(2) 0.1816(4) 0.0272(14) Uani 1 1 d . . . C60 C 0.2896(2) 0.5381(2) 0.2093(4) 0.0287(15) Uani 1 1 d . . . H60 H 0.3119 0.5564 0.1685 0.034 Uiso 1 1 calc R . . C61 C 0.2566(2) 0.5715(2) 0.2490(5) 0.0364(17) Uani 1 1 d . . . H61 H 0.2204 0.5587 0.2534 0.044 Uiso 1 1 calc R . . C62 C 0.2650(2) 0.6289(2) 0.2472(5) 0.0421(18) Uani 1 1 d . . . C63 C 0.2253(3) 0.6647(2) 0.2773(6) 0.058(2) Uani 1 1 d . . . H63 H 0.2328 0.7014 0.2776 0.070 Uiso 1 1 calc R . . C64 C 0.1806(2) 0.6505(3) 0.3038(5) 0.050(2) Uani 1 1 d . . . H64 H 0.1733 0.6138 0.3053 0.060 Uiso 1 1 calc R . . C65 C 0.1411(2) 0.6866(2) 0.3311(6) 0.052(2) Uani 1 1 d . . . C66 C 0.1384(3) 0.7376(3) 0.2957(7) 0.083(3) Uani 1 1 d . . . H66 H 0.1621 0.7482 0.2550 0.099 Uiso 1 1 calc R . . C67 C 0.1012(3) 0.7736(3) 0.3195(7) 0.087(3) Uani 1 1 d . . . H67 H 0.1008 0.8086 0.2963 0.104 Uiso 1 1 calc R . . C68 C 0.0651(3) 0.7589(3) 0.3762(7) 0.075(3) Uani 1 1 d . . . H68 H 0.0399 0.7833 0.3923 0.090 Uiso 1 1 calc R . . C69 C 0.0666(2) 0.7070(2) 0.4093(6) 0.052(2) Uani 1 1 d . . . H69 H 0.0416 0.6960 0.4473 0.063 Uiso 1 1 calc R . . C70 C 0.1041(2) 0.6710(2) 0.3878(5) 0.0443(19) Uani 1 1 d . . . C71 C 0.0968(2) 0.5582(2) 0.3578(5) 0.0335(16) Uani 1 1 d . . . C72 C 0.0596(3) 0.5660(3) 0.2807(5) 0.0438(19) Uani 1 1 d . . . H72 H 0.0396 0.5975 0.2746 0.053 Uiso 1 1 calc R . . C73 C 0.0523(3) 0.5281(3) 0.2143(5) 0.049(2) Uani 1 1 d . . . H73 H 0.0263 0.5334 0.1633 0.059 Uiso 1 1 calc R . . C74 C 0.0816(3) 0.4822(3) 0.2187(5) 0.0447(18) Uani 1 1 d . . . H74 H 0.0772 0.4575 0.1697 0.054 Uiso 1 1 calc R . . C75 C 0.1175(3) 0.4728(3) 0.2961(5) 0.047(2) Uani 1 1 d . . . H75 H 0.1365 0.4407 0.3024 0.057 Uiso 1 1 calc R . . C76 C 0.1253(2) 0.5113(2) 0.3648(5) 0.0426(19) Uani 1 1 d . . . H76 H 0.1504 0.5054 0.4169 0.051 Uiso 1 1 calc R . . C77 C 0.0569(2) 0.6060(2) 0.5162(5) 0.0356(17) Uani 1 1 d . . . C78 C 0.0111(2) 0.5781(2) 0.4901(4) 0.0350(16) Uani 1 1 d . . . H78 H 0.0083 0.5558 0.4378 0.042 Uiso 1 1 calc R . . C79 C -0.0303(2) 0.5825(3) 0.5401(5) 0.0433(18) Uani 1 1 d . . . H79 H -0.0618 0.5639 0.5213 0.052 Uiso 1 1 calc R . . C80 C -0.0261(3) 0.6140(3) 0.6176(5) 0.0459(19) Uani 1 1 d . . . H80 H -0.0546 0.6168 0.6519 0.055 Uiso 1 1 calc R . . C81 C 0.0200(2) 0.6418(2) 0.6455(5) 0.0383(17) Uani 1 1 d . . . H81 H 0.0232 0.6632 0.6989 0.046 Uiso 1 1 calc R . . C82 C 0.0614(3) 0.6376(3) 0.5937(5) 0.0450(19) Uani 1 1 d . . . H82 H 0.0928 0.6566 0.6116 0.054 Uiso 1 1 calc R . . Cu1 Cu 0.31754(3) 0.54406(3) 0.34881(5) 0.0283(2) Uani 1 1 d . . . Cu2 Cu 0.17773(3) 0.54993(3) 0.63853(5) 0.0359(2) Uani 1 1 d . . . O1 O 0.18939(17) 0.66007(19) 0.7413(4) 0.0652(17) Uani 1 1 d . . . O2 O 0.30390(16) 0.64790(16) 0.2203(4) 0.0572(15) Uani 1 1 d . . . O3 O 0.26103(18) 0.4831(2) 0.4092(3) 0.0589(14) Uani 1 1 d . . . O4 O 0.2309(2) 0.4781(2) 0.5879(4) 0.0660(15) Uani 1 1 d . . . P1 P 0.38748(6) 0.61509(6) 0.52656(12) 0.0316(4) Uani 1 1 d . . . P2 P 0.12031(7) 0.47299(8) 0.77681(14) 0.0457(5) Uani 1 1 d . . . P3 P 0.38124(6) 0.45944(6) 0.23406(11) 0.0249(4) Uani 1 1 d . . . P4 P 0.10893(6) 0.60764(6) 0.44575(13) 0.0349(5) Uani 1 1 d . . . S1 S 0.31653(6) 0.60921(6) 0.45551(14) 0.0437(5) Uani 1 1 d . . . S2 S 0.10642(6) 0.49971(7) 0.64904(13) 0.0460(5) Uani 1 1 d . . . S3 S 0.38753(6) 0.49062(6) 0.35996(11) 0.0262(4) Uani 1 1 d . . . S4 S 0.18049(6) 0.60211(6) 0.51496(13) 0.0385(4) Uani 1 1 d . . . F1 F 0.14258(18) 0.3154(2) 0.0773(4) 0.104(2) Uani 1 1 d . . . F2 F 0.0545(2) 0.3130(2) 0.2054(4) 0.121(2) Uani 1 1 d . . . F3 F 0.06389(17) 0.27724(18) 0.0722(4) 0.0853(16) Uani 1 1 d . . . F4 F 0.0739(2) 0.36600(19) 0.0914(5) 0.123(2) Uani 1 1 d . . . F5 F 0.1336(2) 0.3512(2) 0.2151(4) 0.130(3) Uani 1 1 d . . . F6 F 0.1249(2) 0.2640(2) 0.1928(4) 0.111(2) Uani 1 1 d . . . P5 P 0.09879(9) 0.31458(9) 0.1412(2) 0.0715(8) Uani 1 1 d . . . F7 F 0.3628(2) 0.3382(3) 0.9534(4) 0.146(3) Uani 1 1 d . . . F8 F 0.44682(17) 0.31417(17) 0.8206(3) 0.0690(13) Uani 1 1 d . . . F9 F 0.3693(2) 0.2820(3) 0.8325(5) 0.164(3) Uani 1 1 d . . . F10 F 0.3802(3) 0.3674(3) 0.8121(4) 0.163(4) Uani 1 1 d . . . F11 F 0.4388(3) 0.3678(3) 0.9372(5) 0.171(4) Uani 1 1 d . . . F12 F 0.4270(2) 0.28166(19) 0.9549(3) 0.0965(18) Uani 1 1 d . . . P6 P 0.40428(8) 0.32554(8) 0.88630(16) 0.0539(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 C1 0.026(3) 0.024(3) 0.034(4) -0.009(3) 0.006(3) -0.002(3) C2 0.018(3) 0.031(3) 0.055(5) -0.008(4) -0.001(3) 0.008(3) C3 0.037(4) 0.033(4) 0.042(4) -0.001(3) 0.001(3) -0.003(3) C4 0.025(4) 0.046(4) 0.038(4) -0.012(4) 0.006(3) 0.000(3) C5 0.028(4) 0.035(4) 0.041(4) 0.010(3) 0.008(3) 0.009(3) C6 0.025(3) 0.029(3) 0.031(4) 0.000(3) 0.008(3) 0.008(3) C7 0.026(3) 0.017(3) 0.054(5) -0.007(3) 0.011(3) 0.002(3) C8 0.017(3) 0.041(4) 0.060(5) -0.020(4) 0.013(3) -0.007(3) C9 0.042(4) 0.041(4) 0.048(5) -0.004(4) 0.008(4) 0.002(3) C10 0.038(4) 0.035(4) 0.055(5) 0.000(4) 0.017(4) 0.004(3) C11 0.038(4) 0.032(4) 0.077(6) -0.006(4) 0.025(4) 0.002(3) C12 0.022(3) 0.038(4) 0.059(5) -0.016(4) 0.012(3) -0.006(3) C13 0.015(3) 0.028(3) 0.047(4) -0.012(3) 0.003(3) 0.002(3) C14 0.020(3) 0.031(4) 0.056(5) -0.015(3) 0.001(3) 0.003(3) C15 0.019(3) 0.020(3) 0.072(5) -0.006(3) 0.006(3) 0.000(3) C16 0.035(4) 0.027(3) 0.073(6) -0.029(4) 0.006(4) -0.003(3) C17 0.020(4) 0.040(4) 0.088(6) -0.026(4) 0.019(4) -0.006(3) C18 0.020(3) 0.032(4) 0.069(5) -0.024(4) 0.006(3) -0.001(3) C19 0.018(3) 0.027(3) 0.081(6) -0.021(4) 0.017(3) -0.005(3) C20 0.035(4) 0.035(4) 0.076(6) -0.031(4) 0.018(4) -0.009(3) C21 0.027(4) 0.044(4) 0.071(5) -0.030(4) 0.009(4) -0.002(3) C22 0.018(3) 0.045(4) 0.057(5) -0.024(4) 0.007(3) -0.004(3) C23 0.019(3) 0.065(5) 0.047(5) -0.029(4) 0.009(3) 0.001(3) C24 0.026(4) 0.062(5) 0.030(4) -0.005(4) 0.004(3) 0.015(3) C25 0.021(4) 0.092(6) 0.053(5) -0.020(5) -0.003(3) 0.006(4) C26 0.043(5) 0.089(6) 0.043(5) -0.023(5) -0.022(4) 0.039(5) C27 0.037(5) 0.088(6) 0.059(6) -0.006(5) -0.003(4) 0.024(5) C28 0.039(5) 0.101(7) 0.052(5) 0.027(5) -0.002(4) 0.024(5) C29 0.021(4) 0.085(6) 0.029(4) 0.006(4) 0.008(3) 0.009(4) C30 0.021(4) 0.069(5) 0.063(6) 0.043(5) 0.006(4) 0.010(4) C31 0.037(5) 0.059(5) 0.075(6) 0.025(5) 0.002(4) 0.014(4) C32 0.040(5) 0.056(5) 0.134(9) 0.045(6) 0.018(5) 0.009(4) C33 0.070(7) 0.069(7) 0.137(11) 0.049(7) 0.030(7) 0.020(6) C34 0.055(6) 0.087(7) 0.130(10) 0.075(7) 0.041(6) 0.011(5) C35 0.039(5) 0.093(7) 0.111(8) 0.055(6) 0.031(5) 0.031(5) C36 0.023(4) 0.098(6) 0.055(5) 0.038(5) 0.019(4) 0.012(4) C37 0.025(4) 0.091(6) 0.066(6) 0.027(5) 0.005(4) 0.007(4) C38 0.059(6) 0.084(7) 0.089(8) 0.029(6) 0.032(6) 0.030(5) C39 0.091(8) 0.150(10) 0.062(7) 0.044(7) 0.048(6) 0.071(7) C40 0.109(8) 0.173(11) 0.047(6) 0.026(7) 0.032(6) 0.099(8) C41 0.057(5) 0.160(9) 0.039(5) 0.036(6) 0.018(4) 0.064(6) C42 0.027(4) 0.023(3) 0.040(4) -0.007(3) 0.000(3) -0.004(3) C43 0.022(3) 0.026(3) 0.054(5) -0.006(3) -0.002(3) -0.003(3) C44 0.038(4) 0.025(4) 0.074(6) -0.004(4) -0.007(4) -0.004(3) C45 0.044(5) 0.034(4) 0.089(7) -0.025(5) 0.007(5) 0.000(4) C46 0.045(5) 0.060(6) 0.118(9) -0.059(6) 0.029(5) -0.010(4) C47 0.033(4) 0.043(4) 0.048(5) -0.018(4) 0.015(3) -0.003(3) C48 0.018(3) 0.028(3) 0.036(4) -0.005(3) 0.004(3) -0.006(3) C49 0.025(3) 0.036(4) 0.028(4) -0.004(3) -0.001(3) -0.003(3) C50 0.030(4) 0.050(4) 0.048(5) 0.009(4) 0.013(3) -0.013(3) C51 0.050(5) 0.084(6) 0.035(5) 0.007(4) 0.012(4) -0.029(4) C52 0.080(6) 0.152(9) 0.021(4) 0.001(5) 0.003(4) -0.076(6) C53 0.049(5) 0.086(6) 0.035(5) -0.016(4) 0.012(4) -0.045(4) C54 0.025(3) 0.036(4) 0.018(3) -0.005(3) 0.002(3) -0.015(3) C55 0.030(4) 0.048(4) 0.039(4) -0.003(4) 0.006(3) -0.003(3) C56 0.029(4) 0.055(4) 0.056(5) -0.014(4) 0.002(3) -0.025(4) C57 0.019(3) 0.058(5) 0.041(4) -0.003(4) 0.000(3) -0.015(3) C58 0.022(3) 0.053(4) 0.033(4) 0.006(4) 0.002(3) -0.007(3) C59 0.015(3) 0.042(4) 0.024(4) 0.007(3) 0.003(3) 0.005(3) C60 0.020(3) 0.034(3) 0.031(4) 0.015(3) -0.002(3) -0.015(3) C61 0.017(3) 0.030(3) 0.064(5) 0.018(3) 0.011(3) 0.005(3) C62 0.029(4) 0.028(4) 0.072(5) 0.012(4) 0.018(4) 0.001(3) C63 0.031(4) 0.027(4) 0.124(7) 0.039(4) 0.038(4) 0.014(3) C64 0.027(4) 0.031(4) 0.096(6) 0.031(4) 0.023(4) 0.009(3) C65 0.022(4) 0.036(4) 0.101(7) 0.034(4) 0.024(4) 0.012(3) C66 0.034(5) 0.042(4) 0.180(10) 0.060(6) 0.046(5) 0.019(4) C67 0.050(5) 0.051(5) 0.171(10) 0.064(6) 0.062(6) 0.033(4) C68 0.034(4) 0.035(4) 0.163(9) 0.048(5) 0.043(5) 0.015(3) C69 0.026(4) 0.036(4) 0.100(7) 0.019(4) 0.025(4) 0.010(3) C70 0.025(4) 0.031(4) 0.079(6) 0.019(4) 0.013(4) 0.002(3) C71 0.018(3) 0.031(3) 0.054(5) 0.015(3) 0.017(3) 0.003(3) C72 0.036(4) 0.035(4) 0.063(5) 0.012(4) 0.016(4) -0.002(3) C73 0.028(4) 0.066(5) 0.055(5) 0.007(4) 0.013(4) -0.003(4) C74 0.040(4) 0.043(4) 0.055(5) 0.000(4) 0.021(4) -0.008(4) C75 0.047(5) 0.027(4) 0.072(6) 0.007(4) 0.023(4) 0.001(3) C76 0.029(4) 0.028(4) 0.073(6) 0.012(4) 0.018(4) 0.002(3) C77 0.012(3) 0.030(3) 0.068(5) 0.018(4) 0.015(3) 0.002(3) C78 0.029(4) 0.035(4) 0.041(4) 0.010(3) 0.006(3) -0.003(3) C79 0.021(4) 0.055(4) 0.055(5) 0.002(4) 0.008(3) -0.007(3) C80 0.029(4) 0.054(4) 0.058(5) 0.006(4) 0.018(4) -0.002(3) C81 0.028(4) 0.036(4) 0.053(5) -0.002(3) 0.012(3) 0.002(3) C82 0.037(4) 0.034(4) 0.065(5) -0.004(4) 0.011(4) -0.005(3) Cu1 0.0219(4) 0.0249(4) 0.0378(5) -0.0027(4) 0.0033(3) 0.0015(3) Cu2 0.0294(5) 0.0447(5) 0.0334(5) -0.0009(4) 0.0028(4) -0.0135(4) O1 0.029(3) 0.061(3) 0.114(5) -0.048(3) 0.039(3) -0.009(2) O2 0.027(3) 0.034(3) 0.117(5) 0.030(3) 0.034(3) 0.001(2) O3 0.042(3) 0.084(4) 0.053(3) -0.008(3) 0.014(2) -0.021(3) O4 0.065(4) 0.076(4) 0.060(4) 0.004(3) 0.019(3) 0.012(3) P1 0.0138(8) 0.0273(9) 0.0541(12) -0.0164(9) 0.0063(8) -0.0005(7) P2 0.0217(9) 0.0681(13) 0.0468(12) 0.0243(11) 0.0031(8) 0.0015(9) P3 0.0175(8) 0.0254(8) 0.0318(10) -0.0021(8) 0.0032(7) -0.0019(7) P4 0.0208(9) 0.0239(8) 0.0625(13) 0.0122(9) 0.0142(8) 0.0022(7) S1 0.0155(8) 0.0389(10) 0.0750(14) -0.0270(10) -0.0003(8) 0.0027(7) S2 0.0289(9) 0.0603(12) 0.0448(12) 0.0190(10) -0.0099(8) -0.0171(9) S3 0.0224(8) 0.0237(8) 0.0319(10) -0.0007(7) 0.0006(7) 0.0027(6) S4 0.0188(8) 0.0371(9) 0.0613(12) 0.0136(9) 0.0113(8) -0.0016(7) F1 0.059(3) 0.110(4) 0.157(5) -0.069(4) 0.062(3) -0.043(3) F2 0.075(4) 0.154(5) 0.148(5) -0.063(4) 0.073(4) -0.043(4) F3 0.046(3) 0.072(3) 0.140(5) -0.031(3) 0.016(3) -0.024(2) F4 0.098(4) 0.053(3) 0.227(7) -0.039(4) 0.052(5) 0.008(3) F5 0.123(5) 0.139(5) 0.142(5) -0.080(4) 0.069(4) -0.094(4) F6 0.064(4) 0.123(5) 0.141(5) 0.003(4) -0.003(3) -0.039(3) P5 0.0443(13) 0.0540(14) 0.122(2) -0.0360(15) 0.0308(14) -0.0206(11) F7 0.108(5) 0.194(6) 0.162(6) 0.119(5) 0.115(4) 0.107(5) F8 0.066(3) 0.073(3) 0.073(3) -0.001(3) 0.029(3) 0.021(2) F9 0.093(5) 0.258(8) 0.134(6) 0.055(6) -0.012(4) -0.121(5) F10 0.228(8) 0.158(6) 0.125(5) 0.091(5) 0.110(5) 0.156(6) F11 0.225(8) 0.157(6) 0.167(6) -0.104(5) 0.163(6) -0.140(6) F12 0.133(5) 0.083(4) 0.075(4) 0.017(3) 0.019(3) 0.054(3) P6 0.0389(12) 0.0431(11) 0.0855(17) 0.0245(12) 0.0298(11) 0.0052(9) _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 C1 C2 1.379(8) . ? C1 C6 1.394(8) . ? C1 P1 1.810(6) . ? C2 C3 1.383(8) . ? C2 H2 0.9500 . ? C3 C4 1.379(8) . ? C3 H3 0.9500 . ? C4 C5 1.380(8) . ? C4 H4 0.9500 . ? C5 C6 1.369(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.399(8) . ? C7 C8 1.430(9) . ? C7 P1 1.801(6) . ? C8 C9 1.380(9) . ? C8 H8 0.9500 . ? C9 C10 1.361(9) . ? C9 H9 0.9500 . ? C10 C11 1.417(10) . ? C10 H10 0.9500 . ? C11 C12 1.394(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.389(8) . ? C13 C18 1.414(8) . ? C13 P1 1.833(6) . ? C14 C15 1.376(8) . ? C14 H14 0.9500 . ? C15 C16 1.378(8) . ? C15 H15 0.9500 . ? C16 C17 1.399(9) . ? C16 H16 0.9500 . ? C17 C18 1.394(8) . ? C17 H17 0.9500 . ? C18 C19 1.460(8) . ? C19 C20 1.346(8) . ? C19 H19 0.9500 . ? C20 C21 1.490(9) . ? C20 H20 0.9500 . ? C21 O1 1.224(7) . ? C21 C22 1.494(9) . ? C22 C23 1.360(9) . ? C22 Cu2 2.089(6) . ? C22 H22 1.0000 . ? C23 C24 1.492(9) . ? C23 Cu2 2.087(7) . ? C23 H23 1.0000 . ? C24 C29 1.388(9) . ? C24 C25 1.416(9) . ? C25 C26 1.397(10) . ? C25 H25 0.9500 . ? C26 C27 1.374(11) . ? C26 H26 0.9500 . ? C27 C28 1.362(9) . ? C27 H27 0.9500 . ? C28 C29 1.410(10) . ? C28 H28 0.9500 . ? C29 P2 1.806(6) . ? C30 C31 1.375(10) . ? C30 C35 1.417(10) . ? C30 P2 1.819(8) . ? C31 C32 1.399(10) . ? C31 H31 0.9500 . ? C32 C33 1.334(12) . ? C32 H32 0.9500 . ? C33 C34 1.388(13) . ? C33 H33 0.9500 . ? C34 C35 1.437(12) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C41 1.402(11) . ? C36 C37 1.409(10) . ? C36 P2 1.799(8) . ? C37 C38 1.386(11) . ? C37 H37 0.9500 . ? C38 C39 1.350(12) . ? C38 H38 0.9500 . ? C39 C40 1.373(11) . ? C39 H39 0.9500 . ? C40 C41 1.350(11) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.388(8) . ? C42 C47 1.400(8) . ? C42 P3 1.785(6) . ? C43 C44 1.389(8) . ? C43 H43 0.9500 . ? C44 C45 1.369(10) . ? C44 H44 0.9500 . ? C45 C46 1.339(11) . ? C45 H45 0.9500 . ? C46 C47 1.411(10) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.379(8) . ? C48 C53 1.402(9) . ? C48 P3 1.805(6) . ? C49 C50 1.393(8) . ? C49 H49 0.9500 . ? C50 C51 1.349(9) . ? C50 H50 0.9500 . ? C51 C52 1.381(10) . ? C51 H51 0.9500 . ? C52 C53 1.380(9) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C59 1.403(8) . ? C54 C55 1.408(8) . ? C54 P3 1.800(6) . ? C55 C56 1.377(8) . ? C55 H55 0.9500 . ? C56 C57 1.394(9) . ? C56 H56 0.9500 . ? C57 C58 1.373(9) . ? C57 H57 0.9500 . ? C58 C59 1.377(8) . ? C58 H58 0.9500 . ? C59 C60 1.484(8) . ? C60 C61 1.384(8) . ? C60 Cu1 2.091(6) . ? C60 H60 1.0000 . ? C61 C62 1.474(8) . ? C61 Cu1 2.125(6) . ? C61 H61 1.0000 . ? C62 O2 1.225(7) . ? C62 C63 1.481(8) . ? C63 C64 1.319(8) . ? C63 H63 0.9500 . ? C64 C65 1.466(8) . ? C64 H64 0.9500 . ? C65 C66 1.394(8) . ? C65 C70 1.406(8) . ? C66 C67 1.403(10) . ? C66 H66 0.9500 . ? C67 C68 1.383(10) . ? C67 H67 0.9500 . ? C68 C69 1.403(9) . ? C68 H68 0.9500 . ? C69 C70 1.397(8) . ? C69 H69 0.9500 . ? C70 P4 1.816(6) . ? C71 C76 1.395(8) . ? C71 C72 1.402(9) . ? C71 P4 1.800(7) . ? C72 C73 1.367(9) . ? C72 H72 0.9500 . ? C73 C74 1.385(9) . ? C73 H73 0.9500 . ? C74 C75 1.392(10) . ? C74 H74 0.9500 . ? C75 C76 1.400(9) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C82 1.387(9) . ? C77 C78 1.388(8) . ? C77 P4 1.804(6) . ? C78 C79 1.380(8) . ? C78 H78 0.9500 . ? C79 C80 1.385(9) . ? C79 H79 0.9500 . ? C80 C81 1.398(9) . ? C80 H80 0.9500 . ? C81 C82 1.396(9) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? Cu1 S3 2.2488(16) . ? Cu1 S1 2.2826(18) . ? Cu1 O3 2.378(5) . ? Cu2 S4 2.2585(18) . ? Cu2 S2 2.2619(18) . ? Cu2 O4 2.455(5) . ? P1 S1 1.993(2) . ? P2 S2 1.987(3) . ? P3 S3 2.002(2) . ? P4 S4 1.995(2) . ? F1 P5 1.564(5) . ? F2 P5 1.578(5) . ? F3 P5 1.581(5) . ? F4 P5 1.590(6) . ? F5 P5 1.612(6) . ? F6 P5 1.595(6) . ? F7 P6 1.582(5) . ? F8 P6 1.583(4) . ? F9 P6 1.574(7) . ? F10 P6 1.590(5) . ? F11 P6 1.526(6) . ? F12 P6 1.564(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 C2 C1 C6 119.9(6) . . ? C2 C1 P1 118.2(4) . . ? C6 C1 P1 121.5(5) . . ? C1 C2 C3 119.7(6) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 120.5(6) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.5(6) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 120.8(6) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 119.7(6) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C12 C7 C8 119.7(6) . . ? C12 C7 P1 119.7(5) . . ? C8 C7 P1 120.7(5) . . ? C9 C8 C7 119.3(6) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 121.0(7) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 121.0(7) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 119.2(6) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C7 119.8(7) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C14 C13 C18 120.2(5) . . ? C14 C13 P1 120.2(4) . . ? C18 C13 P1 119.3(4) . . ? C15 C14 C13 121.7(6) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 118.8(6) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C15 C16 C17 120.8(6) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 121.0(6) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C13 117.5(6) . . ? C17 C18 C19 119.8(6) . . ? C13 C18 C19 122.7(5) . . ? C20 C19 C18 125.1(6) . . ? C20 C19 H19 117.4 . . ? C18 C19 H19 117.4 . . ? C19 C20 C21 124.8(6) . . ? C19 C20 H20 117.6 . . ? C21 C20 H20 117.6 . . ? O1 C21 C20 118.7(6) . . ? O1 C21 C22 121.2(6) . . ? C20 C21 C22 120.1(6) . . ? C23 C22 C21 119.0(6) . . ? C23 C22 Cu2 70.9(4) . . ? C21 C22 Cu2 104.1(4) . . ? C23 C22 H22 117.5 . . ? C21 C22 H22 117.5 . . ? Cu2 C22 H22 117.5 . . ? C22 C23 C24 124.9(6) . . ? C22 C23 Cu2 71.1(4) . . ? C24 C23 Cu2 110.3(4) . . ? C22 C23 H23 114.2 . . ? C24 C23 H23 114.2 . . ? Cu2 C23 H23 114.2 . . ? C29 C24 C25 118.6(7) . . ? C29 C24 C23 122.4(6) . . ? C25 C24 C23 118.9(7) . . ? C26 C25 C24 119.9(7) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C25 120.0(7) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 121.1(8) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 119.9(8) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C24 C29 C28 120.4(6) . . ? C24 C29 P2 119.4(6) . . ? C28 C29 P2 120.2(6) . . ? C31 C30 C35 121.5(8) . . ? C31 C30 P2 119.9(6) . . ? C35 C30 P2 118.6(7) . . ? C30 C31 C32 119.6(8) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C33 C32 C31 121.5(11) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 120.4(10) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 121.1(9) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C30 C35 C34 115.9(10) . . ? C30 C35 H35 122.0 . . ? C34 C35 H35 122.0 . . ? C41 C36 C37 118.1(8) . . ? C41 C36 P2 122.0(6) . . ? C37 C36 P2 119.8(6) . . ? C38 C37 C36 118.1(8) . . ? C38 C37 H37 121.0 . . ? C36 C37 H37 121.0 . . ? C39 C38 C37 123.5(8) . . ? C39 C38 H38 118.3 . . ? C37 C38 H38 118.3 . . ? C38 C39 C40 117.3(9) . . ? C38 C39 H39 121.3 . . ? C40 C39 H39 121.3 . . ? C41 C40 C39 122.7(9) . . ? C41 C40 H40 118.6 . . ? C39 C40 H40 118.6 . . ? C40 C41 C36 120.2(8) . . ? C40 C41 H41 119.9 . . ? C36 C41 H41 119.9 . . ? C43 C42 C47 118.2(6) . . ? C43 C42 P3 119.8(5) . . ? C47 C42 P3 122.0(5) . . ? C42 C43 C44 120.8(7) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C45 C44 C43 119.6(7) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C46 C45 C44 121.6(7) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C45 C46 C47 119.9(8) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C42 C47 C46 119.8(7) . . ? C42 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C49 C48 C53 118.7(6) . . ? C49 C48 P3 120.7(5) . . ? C53 C48 P3 120.5(4) . . ? C48 C49 C50 120.9(6) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C51 C50 C49 119.7(6) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C50 C51 C52 120.7(7) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C53 C52 C51 120.4(7) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 C48 119.5(6) . . ? C52 C53 H53 120.3 . . ? C48 C53 H53 120.3 . . ? C59 C54 C55 118.8(5) . . ? C59 C54 P3 120.6(4) . . ? C55 C54 P3 120.7(5) . . ? C56 C55 C54 120.4(6) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C55 C56 C57 120.5(6) . . ? C55 C56 H56 119.7 . . ? C57 C56 H56 119.7 . . ? C58 C57 C56 118.7(6) . . ? C58 C57 H57 120.7 . . ? C56 C57 H57 120.7 . . ? C57 C58 C59 122.4(6) . . ? C57 C58 H58 118.8 . . ? C59 C58 H58 118.8 . . ? C58 C59 C54 119.2(6) . . ? C58 C59 C60 120.5(5) . . ? C54 C59 C60 120.3(5) . . ? C61 C60 C59 123.9(5) . . ? C61 C60 Cu1 72.1(4) . . ? C59 C60 Cu1 112.1(4) . . ? C61 C60 H60 113.9 . . ? C59 C60 H60 113.9 . . ? Cu1 C60 H60 113.9 . . ? C60 C61 C62 119.8(5) . . ? C60 C61 Cu1 69.5(3) . . ? C62 C61 Cu1 103.8(4) . . ? C60 C61 H61 117.6 . . ? C62 C61 H61 117.6 . . ? Cu1 C61 H61 117.6 . . ? O2 C62 C61 121.6(6) . . ? O2 C62 C63 119.0(6) . . ? C61 C62 C63 119.4(5) . . ? C64 C63 C62 126.1(6) . . ? C64 C63 H63 117.0 . . ? C62 C63 H63 117.0 . . ? C63 C64 C65 125.4(6) . . ? C63 C64 H64 117.3 . . ? C65 C64 H64 117.3 . . ? C66 C65 C70 118.6(6) . . ? C66 C65 C64 118.7(6) . . ? C70 C65 C64 122.6(6) . . ? C65 C66 C67 120.9(7) . . ? C65 C66 H66 119.5 . . ? C67 C66 H66 119.5 . . ? C68 C67 C66 120.9(7) . . ? C68 C67 H67 119.6 . . ? C66 C67 H67 119.6 . . ? C67 C68 C69 118.2(7) . . ? C67 C68 H68 120.9 . . ? C69 C68 H68 120.9 . . ? C70 C69 C68 121.6(6) . . ? C70 C69 H69 119.2 . . ? C68 C69 H69 119.2 . . ? C69 C70 C65 119.7(6) . . ? C69 C70 P4 118.6(5) . . ? C65 C70 P4 121.2(5) . . ? C76 C71 C72 118.6(7) . . ? C76 C71 P4 120.1(5) . . ? C72 C71 P4 121.3(5) . . ? C73 C72 C71 119.6(6) . . ? C73 C72 H72 120.2 . . ? C71 C72 H72 120.2 . . ? C72 C73 C74 122.4(7) . . ? C72 C73 H73 118.8 . . ? C74 C73 H73 118.8 . . ? C73 C74 C75 118.8(7) . . ? C73 C74 H74 120.6 . . ? C75 C74 H74 120.6 . . ? C74 C75 C76 119.3(6) . . ? C74 C75 H75 120.3 . . ? C76 C75 H75 120.3 . . ? C71 C76 C75 121.1(7) . . ? C71 C76 H76 119.4 . . ? C75 C76 H76 119.4 . . ? C82 C77 C78 119.9(6) . . ? C82 C77 P4 118.1(5) . . ? C78 C77 P4 121.7(6) . . ? C79 C78 C77 120.2(7) . . ? C79 C78 H78 119.9 . . ? C77 C78 H78 119.9 . . ? C78 C79 C80 120.2(6) . . ? C78 C79 H79 119.9 . . ? C80 C79 H79 119.9 . . ? C79 C80 C81 120.3(6) . . ? C79 C80 H80 119.8 . . ? C81 C80 H80 119.8 . . ? C82 C81 C80 119.0(7) . . ? C82 C81 H81 120.5 . . ? C80 C81 H81 120.5 . . ? C77 C82 C81 120.4(6) . . ? C77 C82 H82 119.8 . . ? C81 C82 H82 119.8 . . ? C60 Cu1 C61 38.3(2) . . ? C60 Cu1 S3 101.44(17) . . ? C61 Cu1 S3 139.77(18) . . ? C60 Cu1 S1 134.00(17) . . ? C61 Cu1 S1 99.47(18) . . ? S3 Cu1 S1 117.91(6) . . ? C60 Cu1 O3 99.84(19) . . ? C61 Cu1 O3 92.1(2) . . ? S3 Cu1 O3 96.22(13) . . ? S1 Cu1 O3 98.62(13) . . ? C23 Cu2 C22 38.0(2) . . ? C23 Cu2 S4 135.0(2) . . ? C22 Cu2 S4 98.8(2) . . ? C23 Cu2 S2 100.69(19) . . ? C22 Cu2 S2 138.6(2) . . ? S4 Cu2 S2 119.84(7) . . ? C23 Cu2 O4 98.5(2) . . ? C22 Cu2 O4 94.1(2) . . ? S4 Cu2 O4 96.42(13) . . ? S2 Cu2 O4 95.52(14) . . ? C7 P1 C1 108.8(3) . . ? C7 P1 C13 107.5(3) . . ? C1 P1 C13 105.3(3) . . ? C7 P1 S1 112.3(2) . . ? C1 P1 S1 114.7(2) . . ? C13 P1 S1 107.8(2) . . ? C36 P2 C29 105.2(3) . . ? C36 P2 C30 109.3(4) . . ? C29 P2 C30 107.1(3) . . ? C36 P2 S2 112.1(3) . . ? C29 P2 S2 114.7(2) . . ? C30 P2 S2 108.2(3) . . ? C42 P3 C54 107.3(3) . . ? C42 P3 C48 107.4(3) . . ? C54 P3 C48 106.5(3) . . ? C42 P3 S3 109.9(2) . . ? C54 P3 S3 113.4(2) . . ? C48 P3 S3 112.2(2) . . ? C71 P4 C77 108.9(3) . . ? C71 P4 C70 106.5(3) . . ? C77 P4 C70 106.2(3) . . ? C71 P4 S4 112.4(2) . . ? C77 P4 S4 114.6(2) . . ? C70 P4 S4 107.7(2) . . ? P1 S1 Cu1 108.80(8) . . ? P2 S2 Cu2 102.10(9) . . ? P3 S3 Cu1 101.77(8) . . ? P4 S4 Cu2 109.09(8) . . ? F1 P5 F2 179.3(3) . . ? F1 P5 F3 91.0(3) . . ? F2 P5 F3 88.4(3) . . ? F1 P5 F4 89.6(3) . . ? F2 P5 F4 90.9(4) . . ? F3 P5 F4 91.9(3) . . ? F1 P5 F6 90.1(3) . . ? F2 P5 F6 89.4(4) . . ? F3 P5 F6 89.7(3) . . ? F4 P5 F6 178.3(3) . . ? F1 P5 F5 90.8(3) . . ? F2 P5 F5 89.7(3) . . ? F3 P5 F5 177.5(4) . . ? F4 P5 F5 89.7(4) . . ? F6 P5 F5 88.7(4) . . ? F11 P6 F12 92.1(4) . . ? F11 P6 F9 179.1(3) . . ? F12 P6 F9 88.1(4) . . ? F11 P6 F7 87.2(4) . . ? F12 P6 F7 88.2(3) . . ? F9 P6 F7 93.7(4) . . ? F11 P6 F8 91.2(3) . . ? F12 P6 F8 91.9(3) . . ? F9 P6 F8 87.9(3) . . ? F7 P6 F8 178.4(4) . . ? F11 P6 F10 91.1(5) . . ? F12 P6 F10 176.5(4) . . ? F9 P6 F10 88.7(4) . . ? F7 P6 F10 93.3(3) . . ? F8 P6 F10 86.7(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 C6 C1 C2 C3 -1.2(9) . . . . ? P1 C1 C2 C3 171.6(5) . . . . ? C1 C2 C3 C4 0.9(9) . . . . ? C2 C3 C4 C5 0.2(9) . . . . ? C3 C4 C5 C6 -1.2(9) . . . . ? C4 C5 C6 C1 0.9(9) . . . . ? C2 C1 C6 C5 0.3(9) . . . . ? P1 C1 C6 C5 -172.3(5) . . . . ? C12 C7 C8 C9 1.3(9) . . . . ? P1 C7 C8 C9 -179.3(5) . . . . ? C7 C8 C9 C10 -1.0(9) . . . . ? C8 C9 C10 C11 1.3(10) . . . . ? C9 C10 C11 C12 -2.0(10) . . . . ? C10 C11 C12 C7 2.3(9) . . . . ? C8 C7 C12 C11 -2.0(9) . . . . ? P1 C7 C12 C11 178.6(5) . . . . ? C18 C13 C14 C15 -1.7(10) . . . . ? P1 C13 C14 C15 171.3(5) . . . . ? C13 C14 C15 C16 0.4(10) . . . . ? C14 C15 C16 C17 1.4(11) . . . . ? C15 C16 C17 C18 -2.1(11) . . . . ? C16 C17 C18 C13 0.8(11) . . . . ? C16 C17 C18 C19 179.7(7) . . . . ? C14 C13 C18 C17 1.0(10) . . . . ? P1 C13 C18 C17 -172.0(5) . . . . ? C14 C13 C18 C19 -177.8(6) . . . . ? P1 C13 C18 C19 9.2(9) . . . . ? C17 C18 C19 C20 22.9(11) . . . . ? C13 C18 C19 C20 -158.3(7) . . . . ? C18 C19 C20 C21 -173.2(7) . . . . ? C19 C20 C21 O1 178.2(7) . . . . ? C19 C20 C21 C22 -2.8(11) . . . . ? O1 C21 C22 C23 -15.4(11) . . . . ? C20 C21 C22 C23 165.6(6) . . . . ? O1 C21 C22 Cu2 60.4(8) . . . . ? C20 C21 C22 Cu2 -118.6(6) . . . . ? C21 C22 C23 C24 -162.1(6) . . . . ? Cu2 C22 C23 C24 102.0(6) . . . . ? C21 C22 C23 Cu2 95.9(6) . . . . ? C22 C23 C24 C29 -145.3(7) . . . . ? Cu2 C23 C24 C29 -64.7(7) . . . . ? C22 C23 C24 C25 37.4(10) . . . . ? Cu2 C23 C24 C25 118.0(6) . . . . ? C29 C24 C25 C26 0.2(10) . . . . ? C23 C24 C25 C26 177.6(6) . . . . ? C24 C25 C26 C27 0.3(11) . . . . ? C25 C26 C27 C28 0.0(12) . . . . ? C26 C27 C28 C29 -0.8(12) . . . . ? C25 C24 C29 C28 -1.0(10) . . . . ? C23 C24 C29 C28 -178.4(6) . . . . ? C25 C24 C29 P2 -179.0(5) . . . . ? C23 C24 C29 P2 3.6(9) . . . . ? C27 C28 C29 C24 1.3(11) . . . . ? C27 C28 C29 P2 179.4(6) . . . . ? C35 C30 C31 C32 -1.3(10) . . . . ? P2 C30 C31 C32 176.0(5) . . . . ? C30 C31 C32 C33 2.1(12) . . . . ? C31 C32 C33 C34 -3.2(14) . . . . ? C32 C33 C34 C35 3.6(14) . . . . ? C31 C30 C35 C34 1.6(10) . . . . ? P2 C30 C35 C34 -175.7(6) . . . . ? C33 C34 C35 C30 -2.7(12) . . . . ? C41 C36 C37 C38 -2.9(11) . . . . ? P2 C36 C37 C38 179.1(6) . . . . ? C36 C37 C38 C39 3.1(13) . . . . ? C37 C38 C39 C40 -2.6(15) . . . . ? C38 C39 C40 C41 2.1(17) . . . . ? C39 C40 C41 C36 -2.1(17) . . . . ? C37 C36 C41 C40 2.5(13) . . . . ? P2 C36 C41 C40 -179.6(8) . . . . ? C47 C42 C43 C44 -1.2(9) . . . . ? P3 C42 C43 C44 176.6(5) . . . . ? C42 C43 C44 C45 1.6(9) . . . . ? C43 C44 C45 C46 -0.2(11) . . . . ? C44 C45 C46 C47 -1.6(12) . . . . ? C43 C42 C47 C46 -0.7(9) . . . . ? P3 C42 C47 C46 -178.4(5) . . . . ? C45 C46 C47 C42 2.1(11) . . . . ? C53 C48 C49 C50 -2.2(9) . . . . ? P3 C48 C49 C50 178.0(5) . . . . ? C48 C49 C50 C51 -0.1(10) . . . . ? C49 C50 C51 C52 2.8(12) . . . . ? C50 C51 C52 C53 -3.3(15) . . . . ? C51 C52 C53 C48 1.0(14) . . . . ? C49 C48 C53 C52 1.7(11) . . . . ? P3 C48 C53 C52 -178.5(7) . . . . ? C59 C54 C55 C56 -0.3(9) . . . . ? P3 C54 C55 C56 178.5(5) . . . . ? C54 C55 C56 C57 0.1(10) . . . . ? C55 C56 C57 C58 0.0(10) . . . . ? C56 C57 C58 C59 0.2(10) . . . . ? C57 C58 C59 C54 -0.3(9) . . . . ? C57 C58 C59 C60 177.8(6) . . . . ? C55 C54 C59 C58 0.4(9) . . . . ? P3 C54 C59 C58 -178.4(5) . . . . ? C55 C54 C59 C60 -177.7(5) . . . . ? P3 C54 C59 C60 3.5(8) . . . . ? C58 C59 C60 C61 35.1(9) . . . . ? C54 C59 C60 C61 -146.8(6) . . . . ? C58 C59 C60 Cu1 117.8(5) . . . . ? C54 C59 C60 Cu1 -64.1(6) . . . . ? C59 C60 C61 C62 -160.4(6) . . . . ? Cu1 C60 C61 C62 94.5(6) . . . . ? C59 C60 C61 Cu1 105.1(6) . . . . ? C60 C61 C62 O2 -8.1(11) . . . . ? Cu1 C61 C62 O2 66.0(8) . . . . ? C60 C61 C62 C63 171.1(7) . . . . ? Cu1 C61 C62 C63 -114.9(6) . . . . ? O2 C62 C63 C64 176.6(8) . . . . ? C61 C62 C63 C64 -2.5(13) . . . . ? C62 C63 C64 C65 -178.3(8) . . . . ? C63 C64 C65 C66 26.4(13) . . . . ? C63 C64 C65 C70 -156.9(8) . . . . ? C70 C65 C66 C67 3.0(14) . . . . ? C64 C65 C66 C67 179.8(9) . . . . ? C65 C66 C67 C68 -2.2(16) . . . . ? C66 C67 C68 C69 0.0(15) . . . . ? C67 C68 C69 C70 1.3(14) . . . . ? C68 C69 C70 C65 -0.5(12) . . . . ? C68 C69 C70 P4 171.8(7) . . . . ? C66 C65 C70 C69 -1.7(12) . . . . ? C64 C65 C70 C69 -178.3(7) . . . . ? C66 C65 C70 P4 -173.7(7) . . . . ? C64 C65 C70 P4 9.7(11) . . . . ? C76 C71 C72 C73 -0.3(9) . . . . ? P4 C71 C72 C73 178.4(5) . . . . ? C71 C72 C73 C74 -1.9(10) . . . . ? C72 C73 C74 C75 4.0(10) . . . . ? C73 C74 C75 C76 -3.8(9) . . . . ? C72 C71 C76 C75 0.4(9) . . . . ? P4 C71 C76 C75 -178.3(5) . . . . ? C74 C75 C76 C71 1.6(9) . . . . ? C82 C77 C78 C79 1.4(9) . . . . ? P4 C77 C78 C79 -172.5(5) . . . . ? C77 C78 C79 C80 -1.4(10) . . . . ? C78 C79 C80 C81 0.4(10) . . . . ? C79 C80 C81 C82 0.6(10) . . . . ? C78 C77 C82 C81 -0.4(10) . . . . ? P4 C77 C82 C81 173.7(5) . . . . ? C80 C81 C82 C77 -0.6(10) . . . . ? C59 C60 Cu1 C61 -120.1(6) . . . . ? C61 C60 Cu1 S3 179.2(3) . . . . ? C59 C60 Cu1 S3 59.2(4) . . . . ? C61 C60 Cu1 S1 -31.5(4) . . . . ? C59 C60 Cu1 S1 -151.6(3) . . . . ? C61 C60 Cu1 O3 80.8(3) . . . . ? C59 C60 Cu1 O3 -39.3(4) . . . . ? C62 C61 Cu1 C60 -117.0(6) . . . . ? C60 C61 Cu1 S3 -1.1(5) . . . . ? C62 C61 Cu1 S3 -118.1(4) . . . . ? C60 C61 Cu1 S1 157.6(3) . . . . ? C62 C61 Cu1 S1 40.6(4) . . . . ? C60 C61 Cu1 O3 -103.3(3) . . . . ? C62 C61 Cu1 O3 139.7(4) . . . . ? C24 C23 Cu2 C22 -121.2(6) . . . . ? C22 C23 Cu2 S4 -22.2(5) . . . . ? C24 C23 Cu2 S4 -143.5(4) . . . . ? C22 C23 Cu2 S2 -176.9(4) . . . . ? C24 C23 Cu2 S2 61.8(4) . . . . ? C22 C23 Cu2 O4 85.8(4) . . . . ? C24 C23 Cu2 O4 -35.5(5) . . . . ? C21 C22 Cu2 C23 -116.2(6) . . . . ? C23 C22 Cu2 S4 164.3(4) . . . . ? C21 C22 Cu2 S4 48.1(4) . . . . ? C23 C22 Cu2 S2 4.6(5) . . . . ? C21 C22 Cu2 S2 -111.6(4) . . . . ? C23 C22 Cu2 O4 -98.6(4) . . . . ? C21 C22 Cu2 O4 145.2(4) . . . . ? C12 C7 P1 C1 -104.7(5) . . . . ? C8 C7 P1 C1 75.9(5) . . . . ? C12 C7 P1 C13 141.8(5) . . . . ? C8 C7 P1 C13 -37.6(5) . . . . ? C12 C7 P1 S1 23.4(5) . . . . ? C8 C7 P1 S1 -156.0(4) . . . . ? C2 C1 P1 C7 172.1(4) . . . . ? C6 C1 P1 C7 -15.3(6) . . . . ? C2 C1 P1 C13 -72.9(5) . . . . ? C6 C1 P1 C13 99.7(5) . . . . ? C2 C1 P1 S1 45.4(5) . . . . ? C6 C1 P1 S1 -142.0(4) . . . . ? C14 C13 P1 C7 118.3(5) . . . . ? C18 C13 P1 C7 -68.7(6) . . . . ? C14 C13 P1 C1 2.4(6) . . . . ? C18 C13 P1 C1 175.3(5) . . . . ? C14 C13 P1 S1 -120.5(5) . . . . ? C18 C13 P1 S1 52.5(6) . . . . ? C41 C36 P2 C29 -24.9(8) . . . . ? C37 C36 P2 C29 153.1(6) . . . . ? C41 C36 P2 C30 89.9(7) . . . . ? C37 C36 P2 C30 -92.2(6) . . . . ? C41 C36 P2 S2 -150.2(6) . . . . ? C37 C36 P2 S2 27.7(7) . . . . ? C24 C29 P2 C36 -70.7(6) . . . . ? C28 C29 P2 C36 111.3(6) . . . . ? C24 C29 P2 C30 173.2(6) . . . . ? C28 C29 P2 C30 -4.9(7) . . . . ? C24 C29 P2 S2 53.0(6) . . . . ? C28 C29 P2 S2 -125.0(5) . . . . ? C31 C30 P2 C36 154.6(6) . . . . ? C35 C30 P2 C36 -28.0(6) . . . . ? C31 C30 P2 C29 -91.9(6) . . . . ? C35 C30 P2 C29 85.4(6) . . . . ? C31 C30 P2 S2 32.3(6) . . . . ? C35 C30 P2 S2 -150.3(5) . . . . ? C43 C42 P3 C54 -91.3(5) . . . . ? C47 C42 P3 C54 86.3(5) . . . . ? C43 C42 P3 C48 154.6(5) . . . . ? C47 C42 P3 C48 -27.8(6) . . . . ? C43 C42 P3 S3 32.4(5) . . . . ? C47 C42 P3 S3 -150.0(5) . . . . ? C59 C54 P3 C42 176.4(5) . . . . ? C55 C54 P3 C42 -2.4(6) . . . . ? C59 C54 P3 C48 -68.9(5) . . . . ? C55 C54 P3 C48 112.3(5) . . . . ? C59 C54 P3 S3 54.9(5) . . . . ? C55 C54 P3 S3 -123.8(5) . . . . ? C49 C48 P3 C42 -93.3(5) . . . . ? C53 C48 P3 C42 86.8(6) . . . . ? C49 C48 P3 C54 152.0(5) . . . . ? C53 C48 P3 C54 -27.9(6) . . . . ? C49 C48 P3 S3 27.4(5) . . . . ? C53 C48 P3 S3 -152.4(5) . . . . ? C76 C71 P4 C77 -104.3(5) . . . . ? C72 C71 P4 C77 76.9(5) . . . . ? C76 C71 P4 C70 141.4(5) . . . . ? C72 C71 P4 C70 -37.3(6) . . . . ? C76 C71 P4 S4 23.7(5) . . . . ? C72 C71 P4 S4 -155.0(4) . . . . ? C82 C77 P4 C71 173.7(5) . . . . ? C78 C77 P4 C71 -12.2(6) . . . . ? C82 C77 P4 C70 -71.9(6) . . . . ? C78 C77 P4 C70 102.1(5) . . . . ? C82 C77 P4 S4 46.9(5) . . . . ? C78 C77 P4 S4 -139.1(5) . . . . ? C69 C70 P4 C71 120.1(6) . . . . ? C65 C70 P4 C71 -67.8(7) . . . . ? C69 C70 P4 C77 4.0(7) . . . . ? C65 C70 P4 C77 176.1(6) . . . . ? C69 C70 P4 S4 -119.2(6) . . . . ? C65 C70 P4 S4 52.9(7) . . . . ? C7 P1 S1 Cu1 -82.0(2) . . . . ? C1 P1 S1 Cu1 42.9(2) . . . . ? C13 P1 S1 Cu1 159.7(2) . . . . ? C60 Cu1 S1 P1 -133.9(2) . . . . ? C61 Cu1 S1 P1 -153.03(18) . . . . ? S3 Cu1 S1 P1 11.60(13) . . . . ? O3 Cu1 S1 P1 113.40(16) . . . . ? C36 P2 S2 Cu2 84.6(3) . . . . ? C29 P2 S2 Cu2 -35.3(3) . . . . ? C30 P2 S2 Cu2 -154.8(3) . . . . ? C23 Cu2 S2 P2 -11.2(2) . . . . ? C22 Cu2 S2 P2 -14.0(3) . . . . ? S4 Cu2 S2 P2 -170.77(10) . . . . ? O4 Cu2 S2 P2 88.57(16) . . . . ? C42 P3 S3 Cu1 -159.6(2) . . . . ? C54 P3 S3 Cu1 -39.5(2) . . . . ? C48 P3 S3 Cu1 81.1(2) . . . . ? C60 Cu1 S3 P3 -6.16(17) . . . . ? C61 Cu1 S3 P3 -5.4(3) . . . . ? S1 Cu1 S3 P3 -161.57(8) . . . . ? O3 Cu1 S3 P3 95.22(14) . . . . ? C71 P4 S4 Cu2 -91.6(2) . . . . ? C77 P4 S4 Cu2 33.4(2) . . . . ? C70 P4 S4 Cu2 151.4(3) . . . . ? C23 Cu2 S4 P4 -137.5(3) . . . . ? C22 Cu2 S4 P4 -151.08(19) . . . . ? S2 Cu2 S4 P4 13.60(13) . . . . ? O4 Cu2 S4 P4 113.74(16) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.809 _refine_diff_density_min -1.194 _refine_diff_density_rms 0.108 # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.249 0.250 -0.039 666 247 ' ' 2 0.746 0.313 0.023 259 73 ' ' 3 0.000 0.500 0.000 13 2 ' ' 4 0.254 0.687 -0.023 259 68 ' ' 5 0.751 0.750 -0.009 666 244 ' ' 6 0.254 0.813 0.477 259 69 ' ' 7 0.746 0.187 0.523 259 71 ' ' 8 1.000 1.000 0.500 13 2 ' ' _platon_squeeze_details ; SQUEEZE was used to account for the disordered mixture of dichloromethane and diethyl ether. ; # Attachment '- ijf1015m.cif' data_ijf1015m _database_code_depnum_ccdc_archive 'CCDC 801875' #TrackingRef '- ijf1015m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H32 Cl2 Cu2 O P2 S2' _chemical_formula_sum 'C41 H32 Cl2 Cu2 O P2 S2' _chemical_formula_weight 864.71 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' P P 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.431(3) _cell_length_b 8.9496(10) _cell_length_c 16.2751(18) _cell_angle_alpha 90.00 _cell_angle_beta 115.307(2) _cell_angle_gamma 90.00 _cell_volume 3875.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3979 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.18 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 1.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details 'SADABS v2.10; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _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_% ? _diffrn_reflns_number 18084 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4810 _reflns_number_gt 3180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. There is a small void in the model (volume 31 A^3^). However, the largest peak in the difference map in the void is only 0.62 e/A^3^ so the space is assumed to be empty ; _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^)+(0.0596P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4810 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 C1 C 0.0000 0.5093(5) 0.2500 0.0214(9) Uani 1 2 d S . . C2 C 0.02325(12) 0.5969(4) 0.3361(2) 0.0220(7) Uani 1 1 d . . . H2 H 0.0113(14) 0.691(4) 0.334(2) 0.033(10) Uiso 1 1 d . . . C3 C 0.05312(11) 0.5255(4) 0.4159(2) 0.0206(6) Uani 1 1 d . . . H3 H 0.0611(13) 0.417(4) 0.417(2) 0.028(9) Uiso 1 1 d . . . C4 C 0.06707(12) 0.5878(3) 0.5078(2) 0.0198(6) Uani 1 1 d . . . C5 C 0.03219(12) 0.6759(4) 0.5235(2) 0.0231(7) Uani 1 1 d . . . H5 H 0.0004 0.6966 0.4749 0.028 Uiso 1 1 calc R . . C6 C 0.04377(13) 0.7331(4) 0.6095(2) 0.0249(7) Uani 1 1 d . . . H6 H 0.0197 0.7918 0.6196 0.030 Uiso 1 1 calc R . . C7 C 0.08998(13) 0.7051(4) 0.6803(2) 0.0263(7) Uani 1 1 d . . . H7 H 0.0977 0.7447 0.7389 0.032 Uiso 1 1 calc R . . C8 C 0.12531(12) 0.6192(4) 0.6663(2) 0.0245(7) Uani 1 1 d . . . H8 H 0.1571 0.6008 0.7153 0.029 Uiso 1 1 calc R . . C9 C 0.11423(11) 0.5596(3) 0.5802(2) 0.0201(6) Uani 1 1 d . . . C10 C 0.13664(11) 0.2774(4) 0.5158(2) 0.0209(7) Uani 1 1 d . . . C11 C 0.10360(11) 0.2107(4) 0.5459(2) 0.0209(7) Uani 1 1 d . . . H11 H 0.0953 0.2603 0.5894 0.025 Uiso 1 1 calc R . . C12 C 0.08280(12) 0.0718(4) 0.5123(2) 0.0255(7) Uani 1 1 d . . . H12 H 0.0604 0.0259 0.5329 0.031 Uiso 1 1 calc R . . C13 C 0.09483(13) 0.0011(4) 0.4490(2) 0.0302(8) Uani 1 1 d . . . H13 H 0.0801 -0.0928 0.4250 0.036 Uiso 1 1 calc R . . C14 C 0.12803(14) 0.0651(4) 0.4199(2) 0.0336(8) Uani 1 1 d . . . H14 H 0.1365 0.0142 0.3771 0.040 Uiso 1 1 calc R . . C15 C 0.14922(13) 0.2041(4) 0.4532(2) 0.0283(8) Uani 1 1 d . . . H15 H 0.1721 0.2484 0.4332 0.034 Uiso 1 1 calc R . . C16 C 0.21654(12) 0.4392(4) 0.6616(2) 0.0227(7) Uani 1 1 d . . . C17 C 0.21207(13) 0.3712(4) 0.7354(2) 0.0279(7) Uani 1 1 d . . . H17 H 0.1806 0.3326 0.7285 0.033 Uiso 1 1 calc R . . C18 C 0.25358(13) 0.3605(4) 0.8183(2) 0.0287(8) Uani 1 1 d . . . H18 H 0.2504 0.3176 0.8690 0.034 Uiso 1 1 calc R . . C19 C 0.29961(13) 0.4124(4) 0.8271(2) 0.0305(8) Uani 1 1 d . . . H19 H 0.3281 0.4050 0.8841 0.037 Uiso 1 1 calc R . . C20 C 0.30472(13) 0.4749(4) 0.7538(2) 0.0314(8) Uani 1 1 d . . . H20 H 0.3367 0.5084 0.7604 0.038 Uiso 1 1 calc R . . C21 C 0.26321(12) 0.4889(4) 0.6709(2) 0.0268(7) Uani 1 1 d . . . H21 H 0.2667 0.5322 0.6206 0.032 Uiso 1 1 calc R . . Cl1 Cl 0.09673(3) 0.76495(9) 0.25226(5) 0.0284(2) Uani 1 1 d . . . Cu1 Cu 0.097695(14) 0.61963(4) 0.36132(3) 0.02156(12) Uani 1 1 d . . . O1 O 0.0000 0.3721(3) 0.2500 0.0254(7) Uani 1 2 d S . . P1 P 0.16128(3) 0.46181(9) 0.55641(5) 0.02079(19) Uani 1 1 d . . . S1 S 0.17692(3) 0.57381(10) 0.46475(6) 0.0267(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 C1 0.017(2) 0.025(3) 0.023(2) 0.000 0.0098(18) 0.000 C2 0.0215(16) 0.0186(18) 0.0279(16) -0.0024(13) 0.0124(14) -0.0015(13) C3 0.0179(15) 0.0194(17) 0.0286(16) -0.0019(13) 0.0139(13) -0.0034(13) C4 0.0222(16) 0.0149(16) 0.0241(15) 0.0013(12) 0.0117(13) -0.0029(12) C5 0.0212(16) 0.0192(16) 0.0306(16) 0.0028(14) 0.0126(14) -0.0005(13) C6 0.0283(18) 0.0200(17) 0.0323(17) -0.0015(14) 0.0186(15) -0.0032(14) C7 0.0332(19) 0.0218(18) 0.0284(17) -0.0036(14) 0.0177(15) -0.0044(14) C8 0.0242(17) 0.0216(17) 0.0263(16) 0.0016(14) 0.0094(13) -0.0015(14) C9 0.0206(15) 0.0128(15) 0.0256(15) 0.0000(12) 0.0086(13) -0.0033(12) C10 0.0195(15) 0.0167(16) 0.0234(15) -0.0011(12) 0.0063(13) 0.0006(12) C11 0.0206(16) 0.0183(16) 0.0230(15) 0.0014(13) 0.0085(13) 0.0011(12) C12 0.0221(17) 0.0193(17) 0.0323(17) 0.0041(14) 0.0089(14) -0.0003(13) C13 0.0318(19) 0.0170(17) 0.0343(18) -0.0051(15) 0.0069(15) -0.0017(14) C14 0.045(2) 0.0273(19) 0.0319(18) -0.0080(15) 0.0196(17) -0.0011(16) C15 0.0316(19) 0.0262(19) 0.0305(17) -0.0021(15) 0.0163(15) -0.0026(15) C16 0.0217(16) 0.0159(16) 0.0279(16) -0.0027(13) 0.0080(13) -0.0017(13) C17 0.0242(17) 0.0252(18) 0.0315(17) 0.0003(15) 0.0093(15) -0.0039(14) C18 0.0278(18) 0.0228(19) 0.0296(17) 0.0013(14) 0.0068(15) -0.0011(14) C19 0.0268(18) 0.0214(19) 0.0335(18) -0.0027(14) 0.0035(15) -0.0008(14) C20 0.0193(17) 0.0263(19) 0.043(2) -0.0019(16) 0.0077(15) -0.0028(14) C21 0.0236(17) 0.0221(18) 0.0358(18) 0.0010(14) 0.0136(15) -0.0016(14) Cl1 0.0354(5) 0.0252(4) 0.0292(4) 0.0017(3) 0.0182(4) -0.0050(3) Cu1 0.0230(2) 0.0184(2) 0.0249(2) 0.00006(16) 0.01178(16) -0.00232(16) O1 0.0302(18) 0.0172(17) 0.0281(16) 0.000 0.0117(14) 0.000 P1 0.0182(4) 0.0182(4) 0.0251(4) 0.0004(3) 0.0085(3) -0.0021(3) S1 0.0220(4) 0.0284(5) 0.0314(4) 0.0054(4) 0.0129(4) -0.0028(3) _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 C1 O1 1.228(5) . ? C1 C2 1.492(4) . ? C1 C2 1.492(4) 2 ? C2 C3 1.375(4) . ? C2 Cu1 2.060(3) . ? C2 H2 0.91(4) . ? C3 C4 1.481(4) . ? C3 Cu1 2.053(3) . ? C3 H3 1.00(4) . ? C4 C5 1.401(4) . ? C4 C9 1.407(4) . ? C5 C6 1.389(4) . ? C5 H5 0.9500 . ? C6 C7 1.379(5) . ? C6 H6 0.9500 . ? C7 C8 1.388(5) . ? C7 H7 0.9500 . ? C8 C9 1.401(4) . ? C8 H8 0.9500 . ? C9 P1 1.814(3) . ? C10 C15 1.389(4) . ? C10 C11 1.396(4) . ? C10 P1 1.810(3) . ? C11 C12 1.390(5) . ? C11 H11 0.9500 . ? C12 C13 1.379(5) . ? C12 H12 0.9500 . ? C13 C14 1.378(5) . ? C13 H13 0.9500 . ? C14 C15 1.394(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.389(4) . ? C16 C17 1.402(5) . ? C16 P1 1.799(3) . ? C17 C18 1.383(5) . ? C17 H17 0.9500 . ? C18 C19 1.380(5) . ? C18 H18 0.9500 . ? C19 C20 1.383(5) . ? C19 H19 0.9500 . ? C20 C21 1.386(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? Cl1 Cu1 2.1908(9) . ? Cu1 S1 2.2546(9) . ? P1 S1 2.0072(12) . ? 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 C1 C2 121.7(2) . . ? O1 C1 C2 121.7(2) . 2 ? C2 C1 C2 116.6(4) . 2 ? C3 C2 C1 119.6(3) . . ? C3 C2 Cu1 70.22(18) . . ? C1 C2 Cu1 105.11(17) . . ? C3 C2 H2 123(2) . . ? C1 C2 H2 116(2) . . ? Cu1 C2 H2 106(2) . . ? C2 C3 C4 124.6(3) . . ? C2 C3 Cu1 70.71(18) . . ? C4 C3 Cu1 109.3(2) . . ? C2 C3 H3 121(2) . . ? C4 C3 H3 113(2) . . ? Cu1 C3 H3 102(2) . . ? C5 C4 C9 119.1(3) . . ? C5 C4 C3 119.2(3) . . ? C9 C4 C3 121.8(3) . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C7 C6 C5 120.3(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 120.3(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 120.3(3) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C4 119.5(3) . . ? C8 C9 P1 121.6(2) . . ? C4 C9 P1 118.5(2) . . ? C15 C10 C11 120.0(3) . . ? C15 C10 P1 120.5(2) . . ? C11 C10 P1 119.5(2) . . ? C12 C11 C10 120.0(3) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.2(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C10 C15 C14 119.4(3) . . ? C10 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C21 C16 C17 119.8(3) . . ? C21 C16 P1 121.1(3) . . ? C17 C16 P1 119.1(2) . . ? C18 C17 C16 119.9(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 119.8(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 120.7(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 120.1(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 119.7(3) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? C3 Cu1 C2 39.07(13) . . ? C3 Cu1 Cl1 143.57(10) . . ? C2 Cu1 Cl1 104.65(10) . . ? C3 Cu1 S1 104.51(9) . . ? C2 Cu1 S1 143.46(10) . . ? Cl1 Cu1 S1 111.34(4) . . ? C16 P1 C10 107.62(14) . . ? C16 P1 C9 108.26(14) . . ? C10 P1 C9 107.11(14) . . ? C16 P1 S1 111.23(12) . . ? C10 P1 S1 111.57(11) . . ? C9 P1 S1 110.87(11) . . ? P1 S1 Cu1 98.81(4) . . ? 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 O1 C1 C2 C3 11.8(3) . . . . ? C2 C1 C2 C3 -168.2(3) 2 . . . ? O1 C1 C2 Cu1 87.34(16) . . . . ? C2 C1 C2 Cu1 -92.65(16) 2 . . . ? C1 C2 C3 C4 -162.9(3) . . . . ? Cu1 C2 C3 C4 100.5(3) . . . . ? C1 C2 C3 Cu1 96.6(2) . . . . ? C2 C3 C4 C5 35.0(5) . . . . ? Cu1 C3 C4 C5 114.4(3) . . . . ? C2 C3 C4 C9 -145.8(3) . . . . ? Cu1 C3 C4 C9 -66.4(3) . . . . ? C9 C4 C5 C6 -0.7(5) . . . . ? C3 C4 C5 C6 178.5(3) . . . . ? C4 C5 C6 C7 0.7(5) . . . . ? C5 C6 C7 C8 -0.1(5) . . . . ? C6 C7 C8 C9 -0.3(5) . . . . ? C7 C8 C9 C4 0.3(5) . . . . ? C7 C8 C9 P1 174.1(2) . . . . ? C5 C4 C9 C8 0.3(4) . . . . ? C3 C4 C9 C8 -179.0(3) . . . . ? C5 C4 C9 P1 -173.8(2) . . . . ? C3 C4 C9 P1 7.0(4) . . . . ? C15 C10 C11 C12 -0.8(5) . . . . ? P1 C10 C11 C12 177.3(2) . . . . ? C10 C11 C12 C13 -0.3(5) . . . . ? C11 C12 C13 C14 1.3(5) . . . . ? C12 C13 C14 C15 -1.2(5) . . . . ? C11 C10 C15 C14 0.9(5) . . . . ? P1 C10 C15 C14 -177.2(3) . . . . ? C13 C14 C15 C10 0.1(5) . . . . ? C21 C16 C17 C18 3.2(5) . . . . ? P1 C16 C17 C18 -176.3(3) . . . . ? C16 C17 C18 C19 -2.2(5) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C18 C19 C20 C21 1.3(5) . . . . ? C19 C20 C21 C16 -0.3(5) . . . . ? C17 C16 C21 C20 -1.9(5) . . . . ? P1 C16 C21 C20 177.6(3) . . . . ? C4 C3 Cu1 C2 -121.0(3) . . . . ? C2 C3 Cu1 Cl1 6.7(3) . . . . ? C4 C3 Cu1 Cl1 -114.4(2) . . . . ? C2 C3 Cu1 S1 176.34(17) . . . . ? C4 C3 Cu1 S1 55.3(2) . . . . ? C1 C2 Cu1 C3 -116.5(3) . . . . ? C3 C2 Cu1 Cl1 -175.92(17) . . . . ? C1 C2 Cu1 Cl1 67.5(2) . . . . ? C3 C2 Cu1 S1 -6.0(3) . . . . ? C1 C2 Cu1 S1 -122.5(2) . . . . ? C21 C16 P1 C10 119.2(3) . . . . ? C17 C16 P1 C10 -61.3(3) . . . . ? C21 C16 P1 C9 -125.3(3) . . . . ? C17 C16 P1 C9 54.2(3) . . . . ? C21 C16 P1 S1 -3.3(3) . . . . ? C17 C16 P1 S1 176.2(2) . . . . ? C15 C10 P1 C16 -95.3(3) . . . . ? C11 C10 P1 C16 86.6(3) . . . . ? C15 C10 P1 C9 148.5(3) . . . . ? C11 C10 P1 C9 -29.6(3) . . . . ? C15 C10 P1 S1 27.0(3) . . . . ? C11 C10 P1 S1 -151.1(2) . . . . ? C8 C9 P1 C16 7.2(3) . . . . ? C4 C9 P1 C16 -178.9(2) . . . . ? C8 C9 P1 C10 123.0(3) . . . . ? C4 C9 P1 C10 -63.1(3) . . . . ? C8 C9 P1 S1 -115.0(3) . . . . ? C4 C9 P1 S1 58.9(3) . . . . ? C16 P1 S1 Cu1 -168.08(11) . . . . ? C10 P1 S1 Cu1 71.74(11) . . . . ? C9 P1 S1 Cu1 -47.56(11) . . . . ? C3 Cu1 S1 P1 0.42(11) . . . . ? C2 Cu1 S1 P1 4.29(17) . . . . ? Cl1 Cu1 S1 P1 173.86(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.618 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.104