# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _publ_contact_author_email m.ogden@curtin.edu.au _publ_contact_author_name 'Ogden, Mark' loop_ _publ_author_name 'Mark Light' 'Phil Gale' 'Mark Ogden' data_2008sot1131_complex_4 _database_code_depnum_ccdc_archive 'CCDC 817760' #TrackingRef '- Ogden_Dalton_combined.cif.txt' _chemical_compound_source 'Mark Ogden' _database_code_CSD 8SOT1131 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 Cl Cu N3 S2' _chemical_formula_weight 547.64 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' N N 0.0061 0.0033 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9200(5) _cell_length_b 9.0986(3) _cell_length_c 18.6634(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.731(2) _cell_angle_gamma 90.00 _cell_volume 2533.37(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 20181 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Green' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 1.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8123 _exptl_absorpt_correction_T_max 0.9034 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43572 _diffrn_reflns_av_R_equivalents 0.1149 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5785 _reflns_number_gt 4099 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+2.6335P] 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 5785 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 1.0576(2) 0.8376(4) 0.03907(19) 0.0338(9) Uani 1 1 d . . . H1A H 1.1095 0.7738 0.0477 0.051 Uiso 1 1 calc R . . H1B H 1.0393 0.8826 0.0843 0.051 Uiso 1 1 calc R . . H1C H 1.0736 0.9148 0.0049 0.051 Uiso 1 1 calc R . . C2 C 0.9805(2) 0.7469(4) 0.00840(17) 0.0236(7) Uani 1 1 d . . . H2A H 0.9270 0.8104 0.0029 0.028 Uiso 1 1 calc R . . H2B H 0.9656 0.6676 0.0426 0.028 Uiso 1 1 calc R . . C3 C 1.0023(2) 0.6786(4) -0.06388(16) 0.0227(7) Uani 1 1 d . . . H3A H 1.0593 0.6235 -0.0592 0.027 Uiso 1 1 calc R . . H3B H 1.0116 0.7585 -0.0990 0.027 Uiso 1 1 calc R . . C4 C 0.9300(2) 0.5752(4) -0.09306(17) 0.0220(7) Uani 1 1 d . . . H4A H 0.9511 0.5297 -0.1380 0.026 Uiso 1 1 calc R . . H4B H 0.9197 0.4956 -0.0580 0.026 Uiso 1 1 calc R . . C5 C 0.7739(2) 0.6500(3) -0.06673(15) 0.0188(7) Uani 1 1 d . . . C6 C 0.6955(2) 0.7330(3) -0.08873(15) 0.0186(7) Uani 1 1 d . . . C7 C 0.6728(2) 0.8247(3) -0.14813(15) 0.0187(7) Uani 1 1 d . . . C8 C 0.5810(2) 0.8547(3) -0.14298(15) 0.0172(6) Uani 1 1 d . . . C9 C 0.5518(2) 0.7848(3) -0.07921(15) 0.0181(6) Uani 1 1 d . . . C10 C 0.4706(2) 0.7891(3) -0.03764(15) 0.0199(7) Uani 1 1 d . . . C11 C 0.3224(2) 0.8996(4) -0.01600(17) 0.0273(8) Uani 1 1 d . . . H11A H 0.3378 0.9396 0.0319 0.033 Uiso 1 1 calc R . . H11B H 0.2906 0.8051 -0.0094 0.033 Uiso 1 1 calc R . . C12 C 0.2621(2) 1.0071(4) -0.05614(17) 0.0261(7) Uani 1 1 d . . . H12A H 0.2983 1.0929 -0.0709 0.031 Uiso 1 1 calc R . . H12B H 0.2153 1.0428 -0.0233 0.031 Uiso 1 1 calc R . . C13 C 0.2169(2) 0.9409(4) -0.12227(18) 0.0346(9) Uani 1 1 d . . . H13A H 0.2633 0.8987 -0.1537 0.042 Uiso 1 1 calc R . . H13B H 0.1769 0.8600 -0.1073 0.042 Uiso 1 1 calc R . . C14 C 0.1629(3) 1.0530(6) -0.1642(2) 0.0644(15) Uani 1 1 d . . . H14A H 0.1140 1.0897 -0.1345 0.097 Uiso 1 1 calc R . . H14B H 0.1379 1.0069 -0.2075 0.097 Uiso 1 1 calc R . . H14C H 0.2018 1.1350 -0.1777 0.097 Uiso 1 1 calc R . . C15 C 0.7368(2) 0.8781(3) -0.20294(16) 0.0190(7) Uani 1 1 d . . . C16 C 0.8131(2) 0.9555(4) -0.18186(17) 0.0230(7) Uani 1 1 d . . . H16 H 0.8214 0.9811 -0.1329 0.028 Uiso 1 1 calc R . . C17 C 0.8774(2) 0.9959(4) -0.23146(17) 0.0250(7) Uani 1 1 d . . . H17 H 0.9298 1.0468 -0.2161 0.030 Uiso 1 1 calc R . . C18 C 0.8651(2) 0.9619(4) -0.30329(17) 0.0262(8) Uani 1 1 d . . . H18 H 0.9089 0.9896 -0.3373 0.031 Uiso 1 1 calc R . . C19 C 0.7886(2) 0.8875(4) -0.32534(17) 0.0260(8) Uani 1 1 d . . . H19 H 0.7800 0.8645 -0.3746 0.031 Uiso 1 1 calc R . . C20 C 0.7240(2) 0.8458(4) -0.27590(16) 0.0218(7) Uani 1 1 d . . . H20 H 0.6714 0.7958 -0.2916 0.026 Uiso 1 1 calc R . . C21 C 0.5215(2) 0.9406(4) -0.19236(15) 0.0197(7) Uani 1 1 d . . . C22 C 0.5293(2) 1.0922(4) -0.19910(16) 0.0253(7) Uani 1 1 d . . . H22 H 0.5781 1.1414 -0.1765 0.030 Uiso 1 1 calc R . . C23 C 0.4667(2) 1.1727(4) -0.23836(17) 0.0304(8) Uani 1 1 d . . . H23 H 0.4721 1.2765 -0.2417 0.037 Uiso 1 1 calc R . . C24 C 0.3964(2) 1.1010(4) -0.27261(17) 0.0291(8) Uani 1 1 d . . . H24 H 0.3529 1.1561 -0.2987 0.035 Uiso 1 1 calc R . . C25 C 0.3892(2) 0.9498(4) -0.26906(17) 0.0305(8) Uani 1 1 d . . . H25 H 0.3424 0.9007 -0.2943 0.037 Uiso 1 1 calc R . . C26 C 0.4508(2) 0.8696(4) -0.22839(16) 0.0256(7) Uani 1 1 d . . . H26 H 0.4450 0.7659 -0.2250 0.031 Uiso 1 1 calc R . . N1 N 0.84597(16) 0.6522(3) -0.10712(13) 0.0198(6) Uani 1 1 d . . . H1 H 0.8429 0.7054 -0.1464 0.024 Uiso 1 1 calc R . . N2 N 0.62109(17) 0.7116(3) -0.04871(12) 0.0185(6) Uani 1 1 d . . . N3 N 0.40440(17) 0.8755(3) -0.05699(14) 0.0232(6) Uani 1 1 d . . . H3 H 0.4095 0.9230 -0.0978 0.028 Uiso 1 1 calc R . . S1 S 0.76817(5) 0.54990(9) 0.01075(4) 0.02324(19) Uani 1 1 d . . . S2 S 0.46640(5) 0.68572(10) 0.03898(4) 0.0240(2) Uani 1 1 d . . . Cu1 Cu 0.61573(3) 0.59587(4) 0.035981(18) 0.02030(12) Uani 1 1 d . . . Cl1 Cl 0.61821(6) 0.48629(9) 0.14101(4) 0.0277(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 0.0252(19) 0.039(2) 0.037(2) -0.0069(17) -0.0030(15) -0.0006(17) C2 0.0150(16) 0.0231(18) 0.0326(18) 0.0010(14) -0.0004(13) 0.0030(14) C3 0.0178(16) 0.0248(19) 0.0255(16) 0.0026(13) 0.0023(13) 0.0021(14) C4 0.0178(16) 0.0243(18) 0.0239(16) -0.0017(13) 0.0028(13) 0.0004(14) C5 0.0184(16) 0.0202(17) 0.0179(15) -0.0028(12) -0.0015(12) -0.0023(13) C6 0.0180(16) 0.0190(17) 0.0188(15) -0.0025(12) 0.0031(12) -0.0021(13) C7 0.0189(16) 0.0209(17) 0.0162(14) -0.0025(12) 0.0011(12) -0.0015(13) C8 0.0206(16) 0.0179(16) 0.0132(14) -0.0002(12) -0.0008(12) -0.0014(13) C9 0.0137(15) 0.0227(17) 0.0179(15) 0.0003(12) -0.0009(12) 0.0010(13) C10 0.0207(17) 0.0218(17) 0.0174(15) -0.0010(12) 0.0024(12) 0.0000(14) C11 0.0215(18) 0.037(2) 0.0234(17) 0.0018(14) 0.0054(14) 0.0074(15) C12 0.0182(17) 0.031(2) 0.0293(18) -0.0033(14) 0.0007(13) 0.0051(15) C13 0.0251(19) 0.048(3) 0.0303(19) -0.0100(17) -0.0001(15) 0.0034(17) C14 0.050(3) 0.113(5) 0.030(2) -0.005(2) -0.006(2) 0.036(3) C15 0.0174(16) 0.0191(17) 0.0206(15) 0.0021(12) 0.0023(12) 0.0030(13) C16 0.0242(18) 0.0238(18) 0.0211(16) -0.0006(13) 0.0005(13) 0.0016(14) C17 0.0222(17) 0.0243(19) 0.0286(18) 0.0023(14) 0.0063(14) -0.0022(14) C18 0.0268(19) 0.0227(19) 0.0293(18) 0.0067(14) 0.0096(14) 0.0042(15) C19 0.0312(19) 0.028(2) 0.0190(16) 0.0020(13) 0.0060(14) 0.0052(15) C20 0.0215(17) 0.0209(18) 0.0229(16) 0.0009(13) 0.0013(13) 0.0021(14) C21 0.0204(16) 0.0231(18) 0.0156(15) 0.0019(12) 0.0037(12) 0.0031(14) C22 0.0282(18) 0.0256(19) 0.0222(16) -0.0015(14) 0.0007(14) 0.0009(15) C23 0.039(2) 0.026(2) 0.0267(18) 0.0061(14) 0.0023(16) 0.0079(17) C24 0.0239(18) 0.040(2) 0.0238(17) 0.0137(15) 0.0024(14) 0.0107(16) C25 0.0238(18) 0.043(2) 0.0244(17) 0.0085(15) -0.0026(14) -0.0059(16) C26 0.0250(18) 0.0267(19) 0.0252(17) 0.0061(14) 0.0012(14) 0.0001(15) N1 0.0152(13) 0.0273(15) 0.0170(13) 0.0031(11) 0.0011(10) 0.0026(11) N2 0.0168(13) 0.0212(14) 0.0175(13) 0.0011(10) 0.0019(10) 0.0003(11) N3 0.0187(14) 0.0303(17) 0.0207(13) 0.0062(11) 0.0059(11) 0.0053(12) S1 0.0197(4) 0.0289(5) 0.0211(4) 0.0062(3) 0.0003(3) 0.0022(3) S2 0.0217(4) 0.0318(5) 0.0186(4) 0.0052(3) 0.0042(3) 0.0033(4) Cu1 0.0196(2) 0.0247(2) 0.0166(2) 0.00351(15) 0.00149(15) 0.00073(17) Cl1 0.0318(5) 0.0330(5) 0.0183(4) 0.0066(3) 0.0009(3) 0.0000(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.522(5) . ? C2 C3 1.524(4) . ? C3 C4 1.526(4) . ? C4 N1 1.457(4) . ? C5 N1 1.322(4) . ? C5 C6 1.447(4) . ? C5 S1 1.712(3) . ? C6 N2 1.360(4) . ? C6 C7 1.425(4) . ? C7 C8 1.401(4) . ? C7 C15 1.489(4) . ? C8 C9 1.423(4) . ? C8 C21 1.493(4) . ? C9 N2 1.350(4) . ? C9 C10 1.448(4) . ? C10 N3 1.309(4) . ? C10 S2 1.714(3) . ? C11 N3 1.468(4) . ? C11 C12 1.519(5) . ? C12 C13 1.523(5) . ? C13 C14 1.512(6) . ? C15 C16 1.391(4) . ? C15 C20 1.404(4) . ? C16 C17 1.392(4) . ? C17 C18 1.386(5) . ? C18 C19 1.385(5) . ? C19 C20 1.395(4) . ? C21 C22 1.389(5) . ? C21 C26 1.401(5) . ? C22 C23 1.388(5) . ? C23 C24 1.385(5) . ? C24 C25 1.381(5) . ? C25 C26 1.391(5) . ? N2 Cu1 1.902(2) . ? S1 Cu1 2.3658(9) . ? S2 Cu1 2.3746(9) . ? Cu1 Cl1 2.1991(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 C2 C3 112.7(3) . . ? C2 C3 C4 114.2(3) . . ? N1 C4 C3 111.7(3) . . ? N1 C5 C6 119.4(3) . . ? N1 C5 S1 122.6(2) . . ? C6 C5 S1 117.9(2) . . ? N2 C6 C7 108.9(3) . . ? N2 C6 C5 115.6(3) . . ? C7 C6 C5 135.2(3) . . ? C8 C7 C6 106.5(3) . . ? C8 C7 C15 128.3(3) . . ? C6 C7 C15 125.2(3) . . ? C7 C8 C9 106.3(3) . . ? C7 C8 C21 129.3(3) . . ? C9 C8 C21 124.4(3) . . ? N2 C9 C8 109.4(3) . . ? N2 C9 C10 115.4(3) . . ? C8 C9 C10 134.7(3) . . ? N3 C10 C9 120.1(3) . . ? N3 C10 S2 121.6(2) . . ? C9 C10 S2 118.2(2) . . ? N3 C11 C12 109.3(3) . . ? C11 C12 C13 113.5(3) . . ? C14 C13 C12 112.3(3) . . ? C16 C15 C20 118.8(3) . . ? C16 C15 C7 120.0(3) . . ? C20 C15 C7 121.2(3) . . ? C15 C16 C17 121.0(3) . . ? C18 C17 C16 120.0(3) . . ? C19 C18 C17 119.7(3) . . ? C18 C19 C20 120.7(3) . . ? C19 C20 C15 119.9(3) . . ? C22 C21 C26 118.5(3) . . ? C22 C21 C8 121.7(3) . . ? C26 C21 C8 119.5(3) . . ? C23 C22 C21 121.0(3) . . ? C24 C23 C22 119.7(3) . . ? C25 C24 C23 120.4(3) . . ? C24 C25 C26 119.8(3) . . ? C25 C26 C21 120.5(3) . . ? C5 N1 C4 126.5(3) . . ? C9 N2 C6 108.9(2) . . ? C9 N2 Cu1 125.7(2) . . ? C6 N2 Cu1 125.4(2) . . ? C10 N3 C11 125.2(3) . . ? C5 S1 Cu1 97.61(11) . . ? C10 S2 Cu1 97.19(11) . . ? N2 Cu1 Cl1 172.52(8) . . ? N2 Cu1 S1 83.21(8) . . ? Cl1 Cu1 S1 95.28(3) . . ? N2 Cu1 S2 83.02(8) . . ? Cl1 Cu1 S2 98.06(3) . . ? S1 Cu1 S2 165.99(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 C1 C2 C3 C4 174.6(3) . . . . ? C2 C3 C4 N1 63.3(3) . . . . ? N1 C5 C6 N2 172.8(3) . . . . ? S1 C5 C6 N2 -6.2(4) . . . . ? N1 C5 C6 C7 0.4(5) . . . . ? S1 C5 C6 C7 -178.6(3) . . . . ? N2 C6 C7 C8 -1.3(3) . . . . ? C5 C6 C7 C8 171.4(3) . . . . ? N2 C6 C7 C15 177.6(3) . . . . ? C5 C6 C7 C15 -9.7(6) . . . . ? C6 C7 C8 C9 2.1(3) . . . . ? C15 C7 C8 C9 -176.8(3) . . . . ? C6 C7 C8 C21 -177.5(3) . . . . ? C15 C7 C8 C21 3.6(5) . . . . ? C7 C8 C9 N2 -2.3(3) . . . . ? C21 C8 C9 N2 177.4(3) . . . . ? C7 C8 C9 C10 169.4(3) . . . . ? C21 C8 C9 C10 -11.0(6) . . . . ? N2 C9 C10 N3 169.5(3) . . . . ? C8 C9 C10 N3 -1.7(6) . . . . ? N2 C9 C10 S2 -7.4(4) . . . . ? C8 C9 C10 S2 -178.6(3) . . . . ? N3 C11 C12 C13 73.2(4) . . . . ? C11 C12 C13 C14 -175.8(3) . . . . ? C8 C7 C15 C16 122.9(4) . . . . ? C6 C7 C15 C16 -55.8(4) . . . . ? C8 C7 C15 C20 -60.1(5) . . . . ? C6 C7 C15 C20 121.2(3) . . . . ? C20 C15 C16 C17 -2.3(5) . . . . ? C7 C15 C16 C17 174.7(3) . . . . ? C15 C16 C17 C18 1.4(5) . . . . ? C16 C17 C18 C19 -0.1(5) . . . . ? C17 C18 C19 C20 -0.2(5) . . . . ? C18 C19 C20 C15 -0.7(5) . . . . ? C16 C15 C20 C19 2.0(5) . . . . ? C7 C15 C20 C19 -175.1(3) . . . . ? C7 C8 C21 C22 -69.6(4) . . . . ? C9 C8 C21 C22 110.8(4) . . . . ? C7 C8 C21 C26 116.0(4) . . . . ? C9 C8 C21 C26 -63.6(4) . . . . ? C26 C21 C22 C23 2.4(5) . . . . ? C8 C21 C22 C23 -172.0(3) . . . . ? C21 C22 C23 C24 -1.3(5) . . . . ? C22 C23 C24 C25 -1.3(5) . . . . ? C23 C24 C25 C26 2.7(5) . . . . ? C24 C25 C26 C21 -1.6(5) . . . . ? C22 C21 C26 C25 -1.0(4) . . . . ? C8 C21 C26 C25 173.6(3) . . . . ? C6 C5 N1 C4 -179.9(3) . . . . ? S1 C5 N1 C4 -1.0(4) . . . . ? C3 C4 N1 C5 -102.5(3) . . . . ? C8 C9 N2 C6 1.4(3) . . . . ? C10 C9 N2 C6 -172.0(3) . . . . ? C8 C9 N2 Cu1 -178.1(2) . . . . ? C10 C9 N2 Cu1 8.5(4) . . . . ? C7 C6 N2 C9 -0.1(3) . . . . ? C5 C6 N2 C9 -174.4(3) . . . . ? C7 C6 N2 Cu1 179.5(2) . . . . ? C5 C6 N2 Cu1 5.2(4) . . . . ? C9 C10 N3 C11 -174.2(3) . . . . ? S2 C10 N3 C11 2.6(5) . . . . ? C12 C11 N3 C10 180.0(3) . . . . ? N1 C5 S1 Cu1 -174.7(2) . . . . ? C6 C5 S1 Cu1 4.2(2) . . . . ? N3 C10 S2 Cu1 -173.4(3) . . . . ? C9 C10 S2 Cu1 3.5(3) . . . . ? C9 N2 Cu1 S1 177.6(3) . . . . ? C6 N2 Cu1 S1 -1.9(2) . . . . ? C9 N2 Cu1 S2 -5.0(2) . . . . ? C6 N2 Cu1 S2 175.5(2) . . . . ? C5 S1 Cu1 N2 -1.29(13) . . . . ? C5 S1 Cu1 Cl1 -173.92(11) . . . . ? C5 S1 Cu1 S2 -11.77(19) . . . . ? C10 S2 Cu1 N2 0.40(13) . . . . ? C10 S2 Cu1 Cl1 172.93(11) . . . . ? C10 S2 Cu1 S1 10.88(19) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.394 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.100 #===END data_2009sot0140_complex_6 _database_code_depnum_ccdc_archive 'CCDC 817761' #TrackingRef '- Ogden_Dalton_combined.cif.txt' _chemical_compound_source 'Mark Ogden' _database_code_CSD 9SOT0140 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H18 Cl Cu N3 S2' _chemical_formula_weight 583.58 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' N N 0.0061 0.0033 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3901(2) _cell_length_b 7.73120(10) _cell_length_c 24.4174(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.7560(10) _cell_angle_gamma 90.00 _cell_volume 2305.13(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 23915 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 1.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.963 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 21749 reflections reduced R(int) from 0.1128 to 0.0626 Ratio of minimum to maximum apparent transmission: 0.910843 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21672 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4702 _reflns_number_gt 3992 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.1013P] 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 4702 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.650 _refine_ls_restrained_S_all 1.650 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.76943(3) 0.49234(5) -0.003410(14) 0.01266(12) Uani 1 1 d . . . Cl1 Cl 0.84416(6) 0.54965(10) 0.08177(3) 0.01635(18) Uani 1 1 d . . . S1 S 0.43236(6) 0.23478(10) -0.03680(3) 0.01392(18) Uani 1 1 d . . . S2 S 0.89489(6) 0.76293(10) -0.14670(3) 0.01467(18) Uani 1 1 d . . . N1 N 0.6288(2) 0.3341(3) 0.00541(10) 0.0125(5) Uani 1 1 d . . . N2 N 0.69180(19) 0.4773(3) -0.07584(10) 0.0122(5) Uani 1 1 d . . . N3 N 0.86866(19) 0.6420(3) -0.05092(10) 0.0120(5) Uani 1 1 d . . . C1 C 0.4779(2) 0.1989(4) 0.03347(12) 0.0127(6) Uani 1 1 d . . . C2 C 0.4213(3) 0.1215(4) 0.07227(13) 0.0165(7) Uani 1 1 d . . . H2 H 0.3474 0.0850 0.0620 0.020 Uiso 1 1 calc R . . C3 C 0.4768(3) 0.1004(4) 0.12558(12) 0.0183(7) Uani 1 1 d . . . H3 H 0.4404 0.0485 0.1527 0.022 Uiso 1 1 calc R . . C4 C 0.5860(3) 0.1539(4) 0.14084(12) 0.0170(7) Uani 1 1 d . . . H4 H 0.6229 0.1343 0.1777 0.020 Uiso 1 1 calc R . . C5 C 0.6409(3) 0.2346(4) 0.10316(12) 0.0147(7) Uani 1 1 d . . . H5 H 0.7142 0.2732 0.1140 0.018 Uiso 1 1 calc R . . C6 C 0.5859(2) 0.2580(4) 0.04870(12) 0.0118(6) Uani 1 1 d . . . C7 C 0.5575(2) 0.3268(4) -0.04175(12) 0.0123(6) Uani 1 1 d . . . C8 C 0.5928(2) 0.4017(4) -0.09056(12) 0.0122(6) Uani 1 1 d . . . C9 C 0.5577(2) 0.4234(4) -0.14831(12) 0.0122(6) Uani 1 1 d . . . C10 C 0.6418(2) 0.5215(4) -0.16754(12) 0.0115(6) Uani 1 1 d . . . C11 C 0.7231(2) 0.5506(4) -0.12070(12) 0.0113(6) Uani 1 1 d . . . C12 C 0.8243(2) 0.6435(4) -0.10459(12) 0.0128(6) Uani 1 1 d . . . C13 C 0.9924(2) 0.8153(4) -0.08896(12) 0.0139(7) Uani 1 1 d . . . C14 C 1.0851(2) 0.9177(4) -0.08743(13) 0.0170(7) Uani 1 1 d . . . H14 H 1.1016 0.9709 -0.1201 0.020 Uiso 1 1 calc R . . C15 C 1.1519(3) 0.9390(4) -0.03699(13) 0.0171(7) Uani 1 1 d . . . H15 H 1.2161 1.0077 -0.0347 0.020 Uiso 1 1 calc R . . C16 C 1.1269(2) 0.8607(4) 0.01131(13) 0.0166(7) Uani 1 1 d . . . H16 H 1.1747 0.8768 0.0457 0.020 Uiso 1 1 calc R . . C17 C 1.0334(2) 0.7602(4) 0.00959(13) 0.0149(7) Uani 1 1 d . . . H17 H 1.0165 0.7081 0.0423 0.018 Uiso 1 1 calc R . . C18 C 0.9653(2) 0.7379(4) -0.04136(12) 0.0119(6) Uani 1 1 d . . . C19 C 0.4608(2) 0.3430(4) -0.18225(12) 0.0121(6) Uani 1 1 d . . . C20 C 0.3599(2) 0.3383(4) -0.16452(12) 0.0132(6) Uani 1 1 d . . . H20 H 0.3510 0.3972 -0.1314 0.016 Uiso 1 1 calc R . . C21 C 0.2715(3) 0.2483(4) -0.19465(13) 0.0177(7) Uani 1 1 d . . . H21 H 0.2035 0.2438 -0.1816 0.021 Uiso 1 1 calc R . . C22 C 0.2832(3) 0.1658(4) -0.24352(13) 0.0197(7) Uani 1 1 d . . . H22 H 0.2233 0.1039 -0.2639 0.024 Uiso 1 1 calc R . . C23 C 0.3817(3) 0.1730(4) -0.26284(13) 0.0190(7) Uani 1 1 d . . . H23 H 0.3888 0.1194 -0.2970 0.023 Uiso 1 1 calc R . . C24 C 0.4702(3) 0.2589(4) -0.23214(12) 0.0155(7) Uani 1 1 d . . . H24 H 0.5382 0.2607 -0.2451 0.019 Uiso 1 1 calc R . . C25 C 0.6408(2) 0.5882(4) -0.22456(12) 0.0122(6) Uani 1 1 d . . . C26 C 0.5472(2) 0.6677(4) -0.25357(12) 0.0156(7) Uani 1 1 d . . . H26 H 0.4837 0.6772 -0.2368 0.019 Uiso 1 1 calc R . . C27 C 0.5457(3) 0.7331(4) -0.30667(12) 0.0175(7) Uani 1 1 d . . . H27 H 0.4815 0.7875 -0.3258 0.021 Uiso 1 1 calc R . . C28 C 0.6375(3) 0.7195(4) -0.33173(12) 0.0168(7) Uani 1 1 d . . . H28 H 0.6362 0.7637 -0.3681 0.020 Uiso 1 1 calc R . . C29 C 0.7314(3) 0.6409(4) -0.30350(12) 0.0155(7) Uani 1 1 d . . . H29 H 0.7947 0.6323 -0.3205 0.019 Uiso 1 1 calc R . . C30 C 0.7331(2) 0.5743(4) -0.25022(12) 0.0134(6) Uani 1 1 d . . . H30 H 0.7973 0.5193 -0.2313 0.016 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0124(2) 0.0161(2) 0.00910(19) 0.00010(15) 0.00079(15) -0.00068(15) Cl1 0.0151(4) 0.0236(4) 0.0100(3) -0.0025(3) 0.0012(3) -0.0022(3) S1 0.0124(4) 0.0160(4) 0.0134(4) -0.0001(3) 0.0022(3) -0.0020(3) S2 0.0140(4) 0.0182(4) 0.0115(4) 0.0020(3) 0.0013(3) -0.0029(3) N1 0.0134(13) 0.0146(14) 0.0099(12) -0.0001(11) 0.0034(10) 0.0006(11) N2 0.0071(12) 0.0175(14) 0.0112(12) -0.0007(11) -0.0005(10) -0.0032(10) N3 0.0115(13) 0.0139(14) 0.0101(12) 0.0008(10) 0.0008(10) -0.0009(10) C1 0.0142(16) 0.0121(16) 0.0119(14) 0.0002(13) 0.0023(12) 0.0006(12) C2 0.0142(16) 0.0171(18) 0.0193(16) -0.0028(14) 0.0064(13) -0.0016(13) C3 0.0276(19) 0.0161(18) 0.0137(15) 0.0033(14) 0.0111(14) 0.0012(14) C4 0.0233(18) 0.0167(18) 0.0115(15) -0.0002(13) 0.0041(13) 0.0034(14) C5 0.0165(16) 0.0145(17) 0.0135(15) 0.0007(13) 0.0038(13) 0.0021(13) C6 0.0117(15) 0.0104(16) 0.0143(14) -0.0005(12) 0.0047(12) 0.0038(12) C7 0.0131(16) 0.0118(16) 0.0118(14) -0.0013(12) 0.0019(12) -0.0010(12) C8 0.0105(15) 0.0122(16) 0.0146(15) -0.0006(13) 0.0037(12) 0.0018(12) C9 0.0122(15) 0.0135(17) 0.0115(14) -0.0022(13) 0.0034(12) 0.0005(12) C10 0.0117(15) 0.0123(16) 0.0102(14) -0.0003(12) 0.0009(12) 0.0032(12) C11 0.0095(15) 0.0125(16) 0.0123(14) 0.0010(12) 0.0026(12) 0.0032(12) C12 0.0148(16) 0.0126(17) 0.0119(14) 0.0001(12) 0.0048(12) 0.0026(12) C13 0.0112(15) 0.0154(17) 0.0142(15) -0.0012(13) -0.0005(12) 0.0015(12) C14 0.0152(16) 0.0169(18) 0.0200(16) 0.0019(14) 0.0061(13) 0.0005(13) C15 0.0118(16) 0.0168(17) 0.0222(16) -0.0015(14) 0.0016(13) -0.0027(13) C16 0.0132(16) 0.0203(18) 0.0157(15) -0.0049(14) 0.0011(13) -0.0001(13) C17 0.0132(16) 0.0158(17) 0.0160(15) 0.0012(13) 0.0033(13) 0.0020(13) C18 0.0118(15) 0.0108(16) 0.0124(14) 0.0014(12) -0.0004(12) 0.0033(12) C19 0.0144(16) 0.0110(16) 0.0098(14) 0.0015(12) -0.0011(12) 0.0009(12) C20 0.0138(16) 0.0123(16) 0.0126(14) 0.0003(12) -0.0002(12) 0.0028(12) C21 0.0121(16) 0.0190(18) 0.0212(16) 0.0006(14) 0.0009(13) 0.0015(13) C22 0.0161(17) 0.0168(18) 0.0231(17) -0.0025(14) -0.0061(14) -0.0023(14) C23 0.0246(18) 0.0188(18) 0.0122(15) -0.0040(14) -0.0006(13) 0.0028(14) C24 0.0164(17) 0.0177(18) 0.0124(15) -0.0006(13) 0.0026(13) -0.0004(13) C25 0.0130(15) 0.0126(16) 0.0108(14) -0.0012(13) 0.0017(12) -0.0033(12) C26 0.0135(16) 0.0180(18) 0.0158(15) 0.0002(13) 0.0036(13) -0.0008(13) C27 0.0174(17) 0.0177(18) 0.0153(15) 0.0027(14) -0.0035(13) -0.0009(13) C28 0.0241(18) 0.0160(18) 0.0100(14) 0.0010(13) 0.0020(13) -0.0059(14) C29 0.0160(16) 0.0168(18) 0.0153(15) -0.0035(13) 0.0069(13) -0.0028(13) C30 0.0127(15) 0.0146(17) 0.0122(14) -0.0016(13) -0.0003(12) 0.0001(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.868(2) . ? Cu1 N3 2.163(2) . ? Cu1 N1 2.170(2) . ? Cu1 Cl1 2.1742(8) . ? S1 C7 1.729(3) . ? S1 C1 1.735(3) . ? S2 C12 1.726(3) . ? S2 C13 1.742(3) . ? N1 C7 1.328(4) . ? N1 C6 1.391(4) . ? N2 C11 1.347(4) . ? N2 C8 1.352(4) . ? N3 C12 1.332(4) . ? N3 C18 1.393(4) . ? C1 C6 1.404(4) . ? C1 C2 1.405(4) . ? C2 C3 1.375(4) . ? C3 C4 1.404(4) . ? C4 C5 1.382(4) . ? C5 C6 1.399(4) . ? C7 C8 1.457(4) . ? C8 C9 1.413(4) . ? C9 C10 1.430(4) . ? C9 C19 1.476(4) . ? C10 C11 1.408(4) . ? C10 C25 1.483(4) . ? C11 C12 1.441(4) . ? C13 C14 1.389(4) . ? C13 C18 1.398(4) . ? C14 C15 1.372(4) . ? C15 C16 1.406(4) . ? C16 C17 1.389(4) . ? C17 C18 1.391(4) . ? C19 C20 1.391(4) . ? C19 C24 1.403(4) . ? C20 C21 1.397(4) . ? C21 C22 1.382(4) . ? C22 C23 1.382(4) . ? C23 C24 1.388(4) . ? C25 C26 1.395(4) . ? C25 C30 1.397(4) . ? C26 C27 1.389(4) . ? C27 C28 1.384(4) . ? C28 C29 1.388(4) . ? C29 C30 1.396(4) . ? 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 N2 Cu1 N3 76.92(10) . . ? N2 Cu1 N1 76.44(10) . . ? N3 Cu1 N1 153.36(9) . . ? N2 Cu1 Cl1 170.33(8) . . ? N3 Cu1 Cl1 102.44(7) . . ? N1 Cu1 Cl1 103.83(7) . . ? C7 S1 C1 89.41(14) . . ? C12 S2 C13 89.68(14) . . ? C7 N1 C6 111.0(2) . . ? C7 N1 Cu1 111.40(19) . . ? C6 N1 Cu1 136.9(2) . . ? C11 N2 C8 109.8(2) . . ? C11 N2 Cu1 124.8(2) . . ? C8 N2 Cu1 125.3(2) . . ? C12 N3 C18 111.1(2) . . ? C12 N3 Cu1 110.79(19) . . ? C18 N3 Cu1 138.13(19) . . ? C6 C1 C2 121.5(3) . . ? C6 C1 S1 110.2(2) . . ? C2 C1 S1 128.3(2) . . ? C3 C2 C1 117.6(3) . . ? C2 C3 C4 121.4(3) . . ? C5 C4 C3 121.2(3) . . ? C4 C5 C6 118.4(3) . . ? N1 C6 C5 126.2(3) . . ? N1 C6 C1 113.9(3) . . ? C5 C6 C1 119.9(3) . . ? N1 C7 C8 116.4(3) . . ? N1 C7 S1 115.4(2) . . ? C8 C7 S1 128.1(2) . . ? N2 C8 C9 109.0(3) . . ? N2 C8 C7 109.8(3) . . ? C9 C8 C7 141.2(3) . . ? C8 C9 C10 105.8(3) . . ? C8 C9 C19 126.4(3) . . ? C10 C9 C19 127.4(3) . . ? C11 C10 C9 106.2(2) . . ? C11 C10 C25 126.7(3) . . ? C9 C10 C25 127.0(3) . . ? N2 C11 C10 109.2(3) . . ? N2 C11 C12 110.2(2) . . ? C10 C11 C12 140.4(3) . . ? N3 C12 C11 117.3(3) . . ? N3 C12 S2 115.1(2) . . ? C11 C12 S2 127.6(2) . . ? C14 C13 C18 122.4(3) . . ? C14 C13 S2 127.7(2) . . ? C18 C13 S2 110.0(2) . . ? C15 C14 C13 117.5(3) . . ? C14 C15 C16 121.1(3) . . ? C17 C16 C15 121.1(3) . . ? C16 C17 C18 118.2(3) . . ? C17 C18 N3 126.2(3) . . ? C17 C18 C13 119.7(3) . . ? N3 C18 C13 114.2(3) . . ? C20 C19 C24 118.0(3) . . ? C20 C19 C9 121.7(3) . . ? C24 C19 C9 120.2(3) . . ? C19 C20 C21 121.0(3) . . ? C22 C21 C20 119.8(3) . . ? C21 C22 C23 120.3(3) . . ? C22 C23 C24 119.8(3) . . ? C23 C24 C19 121.1(3) . . ? C26 C25 C30 118.6(3) . . ? C26 C25 C10 120.2(3) . . ? C30 C25 C10 121.2(3) . . ? C27 C26 C25 120.8(3) . . ? C28 C27 C26 120.2(3) . . ? C27 C28 C29 119.7(3) . . ? C28 C29 C30 120.2(3) . . ? C29 C30 C25 120.3(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.490 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.104 #===END data_2009sot0209_complex_5 _database_code_depnum_ccdc_archive 'CCDC 817762' #TrackingRef '- Ogden_Dalton_combined.cif.txt' _chemical_compound_source 'Mark Ogden' _database_code_CSD 9SOT0209 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H22 Cl2 Cu N4 S2' _chemical_formula_weight 661.10 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' N N 0.0061 0.0033 '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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7475(2) _cell_length_b 8.48290(10) _cell_length_c 27.9445(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.7920(10) _cell_angle_gamma 90.00 _cell_volume 2958.03(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7099 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 1.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6596 _exptl_absorpt_correction_T_max 0.8115 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35352 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6752 _reflns_number_gt 5588 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+4.2846P] 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 6752 _refine_ls_number_parameters 375 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.20511(3) 0.05498(4) 0.110630(12) 0.02235(11) Uani 1 1 d . . . Cl1 Cl 0.26078(5) 0.30388(9) 0.11971(3) 0.03255(18) Uani 1 1 d . . . Cl2 Cl 0.29460(6) -0.03233(9) 0.05626(3) 0.03143(17) Uani 1 1 d . . . S1 S -0.17727(5) 0.37659(8) 0.06527(2) 0.02046(15) Uani 1 1 d . . . S2 S 0.13072(6) -0.34755(8) 0.19769(3) 0.02719(16) Uani 1 1 d . . . N1 N 0.02623(17) 0.3759(3) 0.08361(8) 0.0178(4) Uani 1 1 d D . . H901 H 0.0907(16) 0.350(4) 0.0957(11) 0.032(9) Uiso 1 1 d D . . N2 N 0.05340(17) 0.0565(2) 0.12202(8) 0.0174(4) Uani 1 1 d . . . N3 N 0.21810(17) -0.1341(3) 0.15348(8) 0.0218(5) Uani 1 1 d . . . C1 C -0.1107(2) 0.5431(3) 0.04962(9) 0.0195(5) Uani 1 1 d . . . C2 C -0.1539(2) 0.6830(3) 0.02741(10) 0.0229(6) Uani 1 1 d . . . H2 H -0.2292 0.6986 0.0184 0.027 Uiso 1 1 calc R . . C3 C -0.0827(2) 0.7972(3) 0.01910(10) 0.0250(6) Uani 1 1 d . . . H3 H -0.1098 0.8937 0.0043 0.030 Uiso 1 1 calc R . . C4 C 0.0284(2) 0.7752(3) 0.03192(9) 0.0243(6) Uani 1 1 d . . . H4 H 0.0749 0.8565 0.0255 0.029 Uiso 1 1 calc R . . C5 C 0.0713(2) 0.6376(3) 0.05366(9) 0.0217(5) Uani 1 1 d . . . H5 H 0.1466 0.6222 0.0623 0.026 Uiso 1 1 calc R . . C6 C 0.0000(2) 0.5215(3) 0.06252(9) 0.0174(5) Uani 1 1 d . . . C7 C -0.05635(19) 0.2846(3) 0.08764(9) 0.0176(5) Uani 1 1 d . . . C8 C -0.0444(2) 0.1311(3) 0.10924(9) 0.0173(5) Uani 1 1 d . . . C9 C -0.1246(2) 0.0443(3) 0.12629(9) 0.0177(5) Uani 1 1 d . . . C10 C -0.0729(2) -0.0856(3) 0.15151(9) 0.0176(5) Uani 1 1 d . . . C11 C 0.0344(2) -0.0754(3) 0.14726(9) 0.0176(5) Uani 1 1 d . . . C12 C 0.1260(2) -0.1757(3) 0.16412(9) 0.0198(5) Uani 1 1 d . . . C13 C 0.2682(2) -0.3613(4) 0.19952(10) 0.0293(6) Uani 1 1 d . . . C14 C 0.3410(3) -0.4720(4) 0.22325(12) 0.0375(8) Uani 1 1 d . . . H14 H 0.3185 -0.5581 0.2404 0.045 Uiso 1 1 calc R . . C15 C 0.4478(3) -0.4523(4) 0.22093(12) 0.0425(9) Uani 1 1 d . . . H15 H 0.4992 -0.5260 0.2370 0.051 Uiso 1 1 calc R . . C16 C 0.4814(3) -0.3268(4) 0.19558(12) 0.0409(8) Uani 1 1 d . . . H16 H 0.5552 -0.3168 0.1947 0.049 Uiso 1 1 calc R . . C17 C 0.4091(2) -0.2159(4) 0.17149(11) 0.0324(7) Uani 1 1 d . . . H17 H 0.4320 -0.1307 0.1541 0.039 Uiso 1 1 calc R . . C18 C 0.3016(2) -0.2349(3) 0.17387(10) 0.0254(6) Uani 1 1 d . . . C19 C -0.2396(2) 0.0854(3) 0.12082(10) 0.0191(5) Uani 1 1 d . . . C20 C -0.3116(2) 0.0582(4) 0.07699(11) 0.0292(6) Uani 1 1 d . . . H20 H -0.2871 0.0139 0.0500 0.035 Uiso 1 1 calc R . . C21 C -0.4195(2) 0.0957(4) 0.07256(13) 0.0385(8) Uani 1 1 d . . . H21 H -0.4684 0.0767 0.0426 0.046 Uiso 1 1 calc R . . C22 C -0.4558(2) 0.1607(4) 0.11178(13) 0.0364(7) Uani 1 1 d . . . H22 H -0.5294 0.1867 0.1086 0.044 Uiso 1 1 calc R . . C23 C -0.3854(2) 0.1875(4) 0.15510(12) 0.0346(7) Uani 1 1 d . . . H23 H -0.4104 0.2318 0.1819 0.042 Uiso 1 1 calc R . . C24 C -0.2769(2) 0.1498(3) 0.16002(11) 0.0280(6) Uani 1 1 d . . . H24 H -0.2285 0.1682 0.1902 0.034 Uiso 1 1 calc R . . C25 C -0.1214(2) -0.2052(3) 0.17892(9) 0.0192(5) Uani 1 1 d . . . C26 C -0.2007(2) -0.3064(3) 0.15478(10) 0.0240(6) Uani 1 1 d . . . H26 H -0.2240 -0.2995 0.1203 0.029 Uiso 1 1 calc R . . C27 C -0.2462(2) -0.4180(4) 0.18104(12) 0.0321(7) Uani 1 1 d . . . H27 H -0.2995 -0.4880 0.1643 0.039 Uiso 1 1 calc R . . C28 C -0.2140(3) -0.4270(4) 0.23126(13) 0.0385(8) Uani 1 1 d . . . H28 H -0.2447 -0.5037 0.2491 0.046 Uiso 1 1 calc R . . C29 C -0.1371(3) -0.3240(4) 0.25555(11) 0.0378(8) Uani 1 1 d . . . H29 H -0.1164 -0.3284 0.2902 0.045 Uiso 1 1 calc R . . C30 C -0.0898(2) -0.2141(4) 0.22963(10) 0.0284(6) Uani 1 1 d . . . H30 H -0.0360 -0.1451 0.2465 0.034 Uiso 1 1 calc R . . N4 N 0.6105(2) 0.5911(4) 0.05329(12) 0.0487(8) Uani 1 1 d . . . C31 C 0.4120(3) 0.5670(5) 0.06017(15) 0.0494(10) Uani 1 1 d . . . H31A H 0.3794 0.4784 0.0400 0.074 Uiso 1 1 calc R . . H31B H 0.3734 0.6643 0.0488 0.074 Uiso 1 1 calc R . . H31C H 0.4081 0.5478 0.0943 0.074 Uiso 1 1 calc R . . C32 C 0.5232(3) 0.5826(4) 0.05631(11) 0.0335(7) 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 Cu1 0.01787(17) 0.02524(19) 0.02410(18) -0.00073(13) 0.00464(13) 0.00043(13) Cl1 0.0175(3) 0.0283(4) 0.0499(4) -0.0020(3) 0.0023(3) -0.0036(3) Cl2 0.0214(3) 0.0461(4) 0.0279(4) -0.0038(3) 0.0076(3) 0.0027(3) S1 0.0155(3) 0.0192(3) 0.0267(3) 0.0052(3) 0.0043(3) 0.0005(2) S2 0.0296(4) 0.0225(3) 0.0280(4) 0.0048(3) 0.0026(3) 0.0052(3) N1 0.0152(10) 0.0185(11) 0.0194(10) 0.0006(9) 0.0028(9) 0.0001(9) N2 0.0169(10) 0.0174(10) 0.0172(10) -0.0006(8) 0.0019(8) 0.0004(8) N3 0.0188(11) 0.0235(11) 0.0213(11) -0.0027(9) -0.0001(9) 0.0042(9) C1 0.0219(13) 0.0186(12) 0.0182(12) 0.0009(10) 0.0043(10) -0.0025(10) C2 0.0237(13) 0.0218(13) 0.0226(13) 0.0023(11) 0.0033(11) 0.0020(11) C3 0.0363(16) 0.0178(13) 0.0202(13) 0.0016(11) 0.0046(12) -0.0020(12) C4 0.0348(15) 0.0204(13) 0.0186(12) -0.0017(10) 0.0071(11) -0.0093(12) C5 0.0230(13) 0.0238(13) 0.0185(12) -0.0025(11) 0.0050(10) -0.0062(11) C6 0.0222(13) 0.0170(12) 0.0127(11) -0.0009(9) 0.0030(10) -0.0015(10) C7 0.0152(12) 0.0206(12) 0.0177(12) 0.0003(10) 0.0046(10) -0.0006(10) C8 0.0158(12) 0.0185(12) 0.0170(12) 0.0005(10) 0.0020(10) 0.0008(10) C9 0.0182(12) 0.0189(12) 0.0159(11) -0.0012(10) 0.0036(10) 0.0002(10) C10 0.0193(12) 0.0184(12) 0.0149(12) -0.0011(10) 0.0030(10) -0.0010(10) C11 0.0193(12) 0.0183(12) 0.0146(11) -0.0011(10) 0.0022(10) 0.0005(10) C12 0.0230(13) 0.0196(12) 0.0160(12) -0.0027(10) 0.0019(10) 0.0025(10) C13 0.0319(15) 0.0302(15) 0.0236(14) -0.0057(12) 0.0005(12) 0.0067(12) C14 0.0431(19) 0.0348(17) 0.0310(16) 0.0006(13) -0.0009(14) 0.0159(15) C15 0.0405(19) 0.049(2) 0.0326(17) -0.0049(15) -0.0057(15) 0.0248(16) C16 0.0253(16) 0.055(2) 0.0390(18) -0.0084(16) -0.0016(14) 0.0147(15) C17 0.0261(15) 0.0406(17) 0.0286(15) -0.0036(13) 0.0012(12) 0.0075(13) C18 0.0234(14) 0.0309(15) 0.0198(13) -0.0070(11) -0.0004(11) 0.0089(12) C19 0.0164(12) 0.0171(12) 0.0243(13) 0.0047(10) 0.0057(10) -0.0008(10) C20 0.0209(14) 0.0343(16) 0.0314(15) -0.0069(13) 0.0032(12) -0.0017(12) C21 0.0195(14) 0.0464(19) 0.0455(19) -0.0053(16) -0.0032(13) -0.0003(14) C22 0.0183(14) 0.0298(16) 0.063(2) 0.0038(15) 0.0129(14) -0.0009(12) C23 0.0300(16) 0.0346(17) 0.0448(18) 0.0028(14) 0.0207(14) 0.0062(13) C24 0.0276(15) 0.0303(15) 0.0279(14) 0.0027(12) 0.0099(12) 0.0022(12) C25 0.0205(12) 0.0169(12) 0.0217(12) 0.0031(10) 0.0079(10) 0.0048(10) C26 0.0252(14) 0.0226(13) 0.0255(13) 0.0017(11) 0.0088(11) -0.0013(11) C27 0.0282(15) 0.0270(15) 0.0432(18) 0.0071(13) 0.0118(14) -0.0008(12) C28 0.0354(17) 0.0360(17) 0.049(2) 0.0232(15) 0.0198(15) 0.0060(14) C29 0.0458(19) 0.0428(19) 0.0266(15) 0.0165(14) 0.0115(14) 0.0108(16) C30 0.0347(16) 0.0293(15) 0.0209(13) 0.0052(12) 0.0050(12) 0.0045(13) N4 0.0328(16) 0.063(2) 0.0487(18) -0.0059(16) 0.0052(14) -0.0079(15) C31 0.0343(19) 0.060(2) 0.057(2) -0.0205(19) 0.0186(17) -0.0099(17) C32 0.0352(18) 0.0366(17) 0.0277(15) -0.0057(13) 0.0038(13) -0.0056(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.988(2) . ? Cu1 N2 2.023(2) . ? Cu1 Cl2 2.2060(7) . ? Cu1 Cl1 2.2254(8) . ? S1 C7 1.727(3) . ? S1 C1 1.749(3) . ? S2 C12 1.728(3) . ? S2 C13 1.746(3) . ? N1 C7 1.330(3) . ? N1 C6 1.380(3) . ? N2 C11 1.370(3) . ? N2 C8 1.378(3) . ? N3 C12 1.317(3) . ? N3 C18 1.393(3) . ? C1 C6 1.394(4) . ? C1 C2 1.399(4) . ? C2 C3 1.380(4) . ? C3 C4 1.400(4) . ? C4 C5 1.376(4) . ? C5 C6 1.396(4) . ? C7 C8 1.430(4) . ? C8 C9 1.419(3) . ? C9 C10 1.399(4) . ? C9 C19 1.484(3) . ? C10 C11 1.399(3) . ? C10 C25 1.480(3) . ? C11 C12 1.444(4) . ? C13 C14 1.390(4) . ? C13 C18 1.404(4) . ? C14 C15 1.385(5) . ? C15 C16 1.394(5) . ? C16 C17 1.391(4) . ? C17 C18 1.395(4) . ? C19 C24 1.392(4) . ? C19 C20 1.392(4) . ? C20 C21 1.391(4) . ? C21 C22 1.388(5) . ? C22 C23 1.371(5) . ? C23 C24 1.399(4) . ? C25 C26 1.392(4) . ? C25 C30 1.394(4) . ? C26 C27 1.394(4) . ? C27 C28 1.382(5) . ? C28 C29 1.383(5) . ? C29 C30 1.392(4) . ? N4 C32 1.135(4) . ? C31 C32 1.449(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 N3 Cu1 N2 82.82(9) . . ? N3 Cu1 Cl2 98.78(7) . . ? N2 Cu1 Cl2 139.11(6) . . ? N3 Cu1 Cl1 135.35(7) . . ? N2 Cu1 Cl1 105.60(6) . . ? Cl2 Cu1 Cl1 101.50(3) . . ? C7 S1 C1 90.72(12) . . ? C12 S2 C13 89.74(14) . . ? C7 N1 C6 115.5(2) . . ? C11 N2 C8 105.2(2) . . ? C11 N2 Cu1 110.55(16) . . ? C8 N2 Cu1 143.61(17) . . ? C12 N3 C18 112.7(2) . . ? C12 N3 Cu1 112.57(17) . . ? C18 N3 Cu1 134.75(19) . . ? C6 C1 C2 120.8(2) . . ? C6 C1 S1 110.26(19) . . ? C2 C1 S1 128.9(2) . . ? C3 C2 C1 117.2(3) . . ? C2 C3 C4 121.9(3) . . ? C5 C4 C3 121.1(3) . . ? C4 C5 C6 117.5(3) . . ? N1 C6 C1 111.9(2) . . ? N1 C6 C5 126.6(2) . . ? C1 C6 C5 121.5(2) . . ? N1 C7 C8 123.2(2) . . ? N1 C7 S1 111.68(19) . . ? C8 C7 S1 125.08(19) . . ? N2 C8 C9 110.5(2) . . ? N2 C8 C7 122.7(2) . . ? C9 C8 C7 126.3(2) . . ? C10 C9 C8 106.2(2) . . ? C10 C9 C19 126.2(2) . . ? C8 C9 C19 127.5(2) . . ? C9 C10 C11 106.1(2) . . ? C9 C10 C25 126.6(2) . . ? C11 C10 C25 127.2(2) . . ? N2 C11 C10 111.9(2) . . ? N2 C11 C12 115.7(2) . . ? C10 C11 C12 132.4(2) . . ? N3 C12 C11 117.8(2) . . ? N3 C12 S2 114.5(2) . . ? C11 C12 S2 127.6(2) . . ? C14 C13 C18 121.1(3) . . ? C14 C13 S2 128.9(3) . . ? C18 C13 S2 110.0(2) . . ? C15 C14 C13 117.6(3) . . ? C14 C15 C16 121.6(3) . . ? C17 C16 C15 121.4(3) . . ? C16 C17 C18 117.3(3) . . ? N3 C18 C17 125.9(3) . . ? N3 C18 C13 113.0(2) . . ? C17 C18 C13 121.1(3) . . ? C24 C19 C20 119.2(3) . . ? C24 C19 C9 120.0(2) . . ? C20 C19 C9 120.8(2) . . ? C21 C20 C19 120.2(3) . . ? C22 C21 C20 120.2(3) . . ? C23 C22 C21 120.0(3) . . ? C22 C23 C24 120.3(3) . . ? C19 C24 C23 120.1(3) . . ? C26 C25 C30 119.3(2) . . ? C26 C25 C10 120.7(2) . . ? C30 C25 C10 119.9(2) . . ? C25 C26 C27 120.2(3) . . ? C28 C27 C26 120.2(3) . . ? C27 C28 C29 119.8(3) . . ? C28 C29 C30 120.5(3) . . ? C29 C30 C25 120.0(3) . . ? N4 C32 C31 178.4(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H901 Cl1 0.850(18) 2.171(19) 3.016(2) 173(3) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.490 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.104 #===END data_2010acc1015_ligand_3 _database_code_depnum_ccdc_archive 'CCDC 817763' #TrackingRef '- Ogden_Dalton_combined.cif.txt' _chemical_compound_source 'Curtin University, AUS' _database_code_CSD 10AC1015 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H19 N3 S2' _chemical_formula_weight 485.60 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9600(2) _cell_length_b 13.5973(3) _cell_length_c 17.4476(3) _cell_angle_alpha 89.6520(10) _cell_angle_beta 87.1800(10) _cell_angle_gamma 86.9960(10) _cell_volume 2356.79(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 91900 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Slab _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9468 _exptl_absorpt_correction_T_max 0.9925 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40153 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10759 _reflns_number_gt 8548 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Images generated using CrystalMaker: a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd, Oxford, England (www.crystalmaker.com) ; _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.2535P] 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 10759 _refine_ls_number_parameters 639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 S1 S 0.12363(6) 0.73524(4) 0.58120(4) 0.02074(14) Uani 1 1 d . . . S2 S 0.41296(6) 0.20821(5) 0.46292(4) 0.02198(14) Uani 1 1 d . . . N1 N 0.2938(2) 0.70520(15) 0.46443(12) 0.0202(4) Uani 1 1 d . . . N2 N 0.3274(2) 0.50207(15) 0.47941(13) 0.0207(4) Uani 1 1 d . . . H902 H 0.374(3) 0.528(2) 0.4421(17) 0.027(8) Uiso 1 1 d . . . N3 N 0.4709(2) 0.36643(15) 0.38583(12) 0.0223(5) Uani 1 1 d . . . C1 C 0.2651(2) 0.80608(18) 0.46877(14) 0.0190(5) Uani 1 1 d . . . C2 C 0.3192(3) 0.87582(19) 0.41861(15) 0.0230(5) Uani 1 1 d . . . H2 H 0.3815 0.8562 0.3779 0.028 Uiso 1 1 calc R . . C3 C 0.2802(3) 0.97430(19) 0.42962(16) 0.0251(6) Uani 1 1 d . . . H3 H 0.3145 1.0223 0.3952 0.030 Uiso 1 1 calc R . . C4 C 0.1911(3) 1.00408(19) 0.49048(16) 0.0262(6) Uani 1 1 d . . . H4 H 0.1672 1.0721 0.4974 0.031 Uiso 1 1 calc R . . C5 C 0.1375(3) 0.93620(19) 0.54063(15) 0.0246(5) Uani 1 1 d . . . H5 H 0.0767 0.9565 0.5819 0.029 Uiso 1 1 calc R . . C6 C 0.1750(2) 0.83664(18) 0.52917(14) 0.0187(5) Uani 1 1 d . . . C7 C 0.2267(2) 0.66011(18) 0.51916(14) 0.0188(5) Uani 1 1 d . . . C8 C 0.2396(2) 0.55404(18) 0.52789(14) 0.0195(5) Uani 1 1 d . . . C9 C 0.1816(2) 0.48817(18) 0.57928(14) 0.0197(5) Uani 1 1 d . . . C10 C 0.2393(2) 0.39312(18) 0.56084(14) 0.0193(5) Uani 1 1 d . . . C11 C 0.3282(3) 0.40426(18) 0.49773(14) 0.0203(5) Uani 1 1 d . . . C12 C 0.4058(2) 0.33573(18) 0.44750(14) 0.0200(5) Uani 1 1 d . . . C13 C 0.5137(2) 0.19439(19) 0.37924(15) 0.0212(5) Uani 1 1 d . . . C14 C 0.5709(3) 0.10835(19) 0.34523(16) 0.0245(6) Uani 1 1 d . . . H14 H 0.5597 0.0460 0.3688 0.029 Uiso 1 1 calc R . . C15 C 0.6440(3) 0.1164(2) 0.27650(16) 0.0260(6) Uani 1 1 d . . . H15 H 0.6829 0.0587 0.2522 0.031 Uiso 1 1 calc R . . C16 C 0.6615(3) 0.2082(2) 0.24213(16) 0.0277(6) Uani 1 1 d . . . H16 H 0.7114 0.2118 0.1944 0.033 Uiso 1 1 calc R . . C17 C 0.6078(3) 0.2937(2) 0.27615(16) 0.0268(6) Uani 1 1 d . . . H17 H 0.6218 0.3559 0.2529 0.032 Uiso 1 1 calc R . . C18 C 0.5323(2) 0.28712(18) 0.34565(14) 0.0212(5) Uani 1 1 d . . . C19 C 0.0815(3) 0.51402(18) 0.64311(14) 0.0204(5) Uani 1 1 d . . . C20 C -0.0489(3) 0.54754(19) 0.62863(15) 0.0237(5) Uani 1 1 d . . . H20 H -0.0764 0.5511 0.5773 0.028 Uiso 1 1 calc R . . C21 C -0.1395(3) 0.5759(2) 0.68835(17) 0.0292(6) Uani 1 1 d . . . H21 H -0.2283 0.5991 0.6776 0.035 Uiso 1 1 calc R . . C22 C -0.1012(3) 0.5704(2) 0.76335(17) 0.0331(7) Uani 1 1 d . . . H22 H -0.1626 0.5911 0.8042 0.040 Uiso 1 1 calc R . . C23 C 0.0274(3) 0.5347(2) 0.77844(16) 0.0343(7) Uani 1 1 d . . . H23 H 0.0537 0.5295 0.8300 0.041 Uiso 1 1 calc R . . C24 C 0.1184(3) 0.5062(2) 0.71865(15) 0.0279(6) Uani 1 1 d . . . H24 H 0.2063 0.4812 0.7296 0.033 Uiso 1 1 calc R . . C25 C 0.2071(3) 0.30019(18) 0.60112(14) 0.0203(5) Uani 1 1 d . . . C26 C 0.0755(3) 0.26805(19) 0.60321(15) 0.0253(6) Uani 1 1 d . . . H26 H 0.0068 0.3054 0.5785 0.030 Uiso 1 1 calc R . . C27 C 0.0458(3) 0.1813(2) 0.64156(16) 0.0282(6) Uani 1 1 d . . . H27 H -0.0433 0.1595 0.6428 0.034 Uiso 1 1 calc R . . C28 C 0.1449(3) 0.12659(19) 0.67792(15) 0.0265(6) Uani 1 1 d . . . H28 H 0.1240 0.0672 0.7037 0.032 Uiso 1 1 calc R . . C29 C 0.2749(3) 0.15855(19) 0.67674(15) 0.0256(6) Uani 1 1 d . . . H29 H 0.3430 0.1212 0.7020 0.031 Uiso 1 1 calc R . . C30 C 0.3058(3) 0.24520(19) 0.63869(14) 0.0235(5) Uani 1 1 d . . . H30 H 0.3949 0.2670 0.6383 0.028 Uiso 1 1 calc R . . S3 S 0.68248(6) 0.27920(5) -0.03879(4) 0.02125(14) Uani 1 1 d . . . S4 S 0.31922(7) -0.11188(5) 0.21416(4) 0.02391(15) Uani 1 1 d . . . N4 N 0.8043(2) 0.11310(15) -0.00091(12) 0.0202(4) Uani 1 1 d . . . N5 N 0.5882(2) 0.03506(16) 0.08137(12) 0.0202(4) Uani 1 1 d . . . H905 H 0.651(3) -0.007(2) 0.0680(18) 0.039(9) Uiso 1 1 d . . . N6 N 0.5529(2) -0.15289(15) 0.14433(12) 0.0211(4) Uani 1 1 d . . . C31 C 0.8929(2) 0.16124(18) -0.05036(14) 0.0192(5) Uani 1 1 d . . . C32 C 1.0214(3) 0.1245(2) -0.07538(15) 0.0242(5) Uani 1 1 d . . . H32 H 1.0578 0.0639 -0.0561 0.029 Uiso 1 1 calc R . . C33 C 1.0943(3) 0.1786(2) -0.12881(15) 0.0263(6) Uani 1 1 d . . . H33 H 1.1815 0.1544 -0.1464 0.032 Uiso 1 1 calc R . . C34 C 1.0419(3) 0.2682(2) -0.15735(15) 0.0268(6) Uani 1 1 d . . . H34 H 1.0933 0.3030 -0.1948 0.032 Uiso 1 1 calc R . . C35 C 0.9169(3) 0.3070(2) -0.13196(15) 0.0240(5) Uani 1 1 d . . . H35 H 0.8819 0.3685 -0.1506 0.029 Uiso 1 1 calc R . . C36 C 0.8440(2) 0.25275(18) -0.07806(14) 0.0200(5) Uani 1 1 d . . . C37 C 0.6910(2) 0.16567(18) 0.00919(14) 0.0193(5) Uani 1 1 d . . . C38 C 0.5783(2) 0.13027(18) 0.05461(13) 0.0184(5) Uani 1 1 d . . . C39 C 0.4526(2) 0.17148(18) 0.07937(14) 0.0187(5) Uani 1 1 d . . . C40 C 0.3867(2) 0.09765(18) 0.12270(14) 0.0184(5) Uani 1 1 d . . . C41 C 0.4723(2) 0.01419(18) 0.12242(14) 0.0189(5) Uani 1 1 d . . . C42 C 0.4603(2) -0.08255(18) 0.15573(14) 0.0198(5) Uani 1 1 d . . . C43 C 0.3914(3) -0.22998(19) 0.22378(14) 0.0231(5) Uani 1 1 d . . . C44 C 0.3397(3) -0.3104(2) 0.26353(16) 0.0293(6) Uani 1 1 d . . . H44 H 0.2559 -0.3044 0.2920 0.035 Uiso 1 1 calc R . . C45 C 0.4142(3) -0.3985(2) 0.25998(17) 0.0330(7) Uani 1 1 d . . . H45 H 0.3823 -0.4538 0.2875 0.040 Uiso 1 1 calc R . . C46 C 0.5361(3) -0.4082(2) 0.21670(18) 0.0336(7) Uani 1 1 d . . . H46 H 0.5839 -0.4705 0.2140 0.040 Uiso 1 1 calc R . . C47 C 0.5882(3) -0.3290(2) 0.17778(17) 0.0286(6) Uani 1 1 d . . . H47 H 0.6715 -0.3359 0.1490 0.034 Uiso 1 1 calc R . . C48 C 0.5151(3) -0.23829(19) 0.18186(15) 0.0227(5) Uani 1 1 d . . . C49 C 0.3913(3) 0.27096(18) 0.06347(14) 0.0196(5) Uani 1 1 d . . . C50 C 0.2695(3) 0.2776(2) 0.02713(15) 0.0263(6) Uani 1 1 d . . . H50 H 0.2290 0.2192 0.0126 0.032 Uiso 1 1 calc R . . C51 C 0.2069(3) 0.3688(2) 0.01204(16) 0.0300(6) Uani 1 1 d . . . H51 H 0.1235 0.3725 -0.0123 0.036 Uiso 1 1 calc R . . C52 C 0.2657(3) 0.4542(2) 0.03231(16) 0.0289(6) Uani 1 1 d . . . H52 H 0.2233 0.5166 0.0213 0.035 Uiso 1 1 calc R . . C53 C 0.3860(3) 0.44877(19) 0.06846(15) 0.0270(6) Uani 1 1 d . . . H53 H 0.4267 0.5073 0.0823 0.032 Uiso 1 1 calc R . . C54 C 0.4475(3) 0.35746(19) 0.08462(14) 0.0231(5) Uani 1 1 d . . . H54 H 0.5293 0.3541 0.1105 0.028 Uiso 1 1 calc R . . C55 C 0.2555(2) 0.11091(18) 0.16659(14) 0.0193(5) Uani 1 1 d . . . C56 C 0.1363(3) 0.0835(2) 0.13708(16) 0.0273(6) Uani 1 1 d . . . H56 H 0.1371 0.0555 0.0873 0.033 Uiso 1 1 calc R . . C57 C 0.0159(3) 0.0968(2) 0.17989(17) 0.0310(6) Uani 1 1 d . . . H57 H -0.0656 0.0786 0.1591 0.037 Uiso 1 1 calc R . . C58 C 0.0137(3) 0.1365(2) 0.25305(16) 0.0273(6) Uani 1 1 d . . . H58 H -0.0689 0.1451 0.2825 0.033 Uiso 1 1 calc R . . C59 C 0.1316(3) 0.1633(2) 0.28256(16) 0.0298(6) Uani 1 1 d . . . H59 H 0.1306 0.1901 0.3328 0.036 Uiso 1 1 calc R . . C60 C 0.2523(3) 0.1515(2) 0.23964(15) 0.0252(6) Uani 1 1 d . . . H60 H 0.3332 0.1712 0.2603 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0233(3) 0.0163(3) 0.0220(3) -0.0007(2) 0.0036(2) 0.0008(2) S2 0.0221(3) 0.0155(3) 0.0279(3) -0.0006(2) 0.0014(3) 0.0006(2) N1 0.0195(11) 0.0169(10) 0.0239(11) -0.0004(8) -0.0003(8) 0.0003(8) N2 0.0235(11) 0.0157(10) 0.0224(11) -0.0006(9) 0.0031(9) -0.0002(9) N3 0.0218(11) 0.0174(10) 0.0274(12) 0.0011(9) -0.0008(9) 0.0021(8) C1 0.0195(12) 0.0177(12) 0.0199(12) -0.0015(9) -0.0030(9) 0.0002(9) C2 0.0230(13) 0.0221(13) 0.0238(13) -0.0003(10) 0.0005(10) -0.0011(10) C3 0.0258(14) 0.0187(13) 0.0310(14) 0.0028(11) -0.0011(11) -0.0041(10) C4 0.0248(14) 0.0158(12) 0.0381(15) -0.0007(11) -0.0032(11) -0.0002(10) C5 0.0249(13) 0.0191(13) 0.0293(14) -0.0035(11) 0.0006(11) 0.0003(10) C6 0.0186(12) 0.0177(12) 0.0202(12) 0.0001(9) -0.0033(9) -0.0030(9) C7 0.0193(12) 0.0180(12) 0.0189(12) -0.0019(9) -0.0015(9) 0.0016(10) C8 0.0182(12) 0.0191(12) 0.0214(12) -0.0005(10) -0.0014(10) -0.0005(10) C9 0.0186(12) 0.0169(12) 0.0239(13) -0.0004(10) -0.0040(10) -0.0002(10) C10 0.0185(12) 0.0170(12) 0.0227(12) -0.0004(10) -0.0035(10) -0.0003(9) C11 0.0212(13) 0.0141(12) 0.0259(13) -0.0010(10) -0.0040(10) -0.0002(10) C12 0.0183(12) 0.0172(12) 0.0245(13) 0.0001(10) -0.0036(10) -0.0003(10) C13 0.0166(12) 0.0206(12) 0.0265(13) -0.0011(10) -0.0033(10) 0.0007(10) C14 0.0206(13) 0.0194(13) 0.0335(15) -0.0023(11) -0.0041(11) 0.0010(10) C15 0.0202(13) 0.0258(14) 0.0315(14) -0.0080(11) -0.0025(11) 0.0062(11) C16 0.0252(14) 0.0313(15) 0.0256(14) -0.0009(11) 0.0010(11) 0.0042(11) C17 0.0256(14) 0.0251(14) 0.0292(14) 0.0036(11) -0.0022(11) 0.0023(11) C18 0.0192(12) 0.0203(12) 0.0243(13) -0.0018(10) -0.0051(10) 0.0005(10) C19 0.0236(13) 0.0138(11) 0.0237(13) 0.0005(10) 0.0008(10) -0.0018(10) C20 0.0225(13) 0.0239(13) 0.0245(13) 0.0017(11) 0.0008(10) -0.0013(10) C21 0.0213(13) 0.0277(15) 0.0375(16) 0.0073(12) 0.0053(11) 0.0012(11) C22 0.0357(16) 0.0316(16) 0.0306(15) 0.0010(12) 0.0126(12) -0.0021(13) C23 0.0426(18) 0.0403(17) 0.0197(14) 0.0014(12) 0.0012(12) -0.0021(14) C24 0.0252(14) 0.0315(15) 0.0270(14) 0.0012(12) -0.0037(11) 0.0006(11) C25 0.0241(13) 0.0162(12) 0.0204(12) -0.0010(10) -0.0008(10) 0.0002(10) C26 0.0259(14) 0.0227(13) 0.0276(14) 0.0016(11) -0.0064(11) 0.0011(11) C27 0.0266(14) 0.0267(14) 0.0316(15) 0.0013(12) 0.0011(11) -0.0073(11) C28 0.0408(16) 0.0174(13) 0.0213(13) 0.0000(10) -0.0008(11) -0.0035(11) C29 0.0362(15) 0.0197(13) 0.0208(13) 0.0016(10) -0.0050(11) 0.0043(11) C30 0.0260(14) 0.0216(13) 0.0228(13) -0.0023(10) -0.0040(10) 0.0018(10) S3 0.0196(3) 0.0189(3) 0.0248(3) 0.0034(2) 0.0021(2) -0.0005(2) S4 0.0250(3) 0.0204(3) 0.0255(3) 0.0027(3) 0.0064(3) -0.0007(3) N4 0.0184(10) 0.0217(11) 0.0203(10) -0.0005(8) 0.0017(8) -0.0019(8) N5 0.0208(11) 0.0177(11) 0.0215(11) 0.0005(8) 0.0029(9) 0.0010(9) N6 0.0181(10) 0.0199(11) 0.0252(11) 0.0010(9) -0.0022(8) -0.0007(8) C31 0.0183(12) 0.0206(12) 0.0192(12) -0.0005(10) -0.0019(9) -0.0041(10) C32 0.0199(13) 0.0275(14) 0.0251(13) -0.0014(11) -0.0016(10) 0.0014(11) C33 0.0175(13) 0.0359(15) 0.0255(14) -0.0020(12) 0.0016(10) -0.0045(11) C34 0.0243(14) 0.0318(15) 0.0248(14) 0.0019(11) 0.0039(11) -0.0096(11) C35 0.0228(13) 0.0247(13) 0.0247(13) 0.0027(11) -0.0004(10) -0.0052(11) C36 0.0187(12) 0.0193(12) 0.0220(12) -0.0020(10) 0.0007(10) -0.0025(10) C37 0.0200(12) 0.0201(12) 0.0179(12) -0.0017(9) -0.0016(9) -0.0022(10) C38 0.0193(12) 0.0186(12) 0.0173(12) 0.0008(9) -0.0008(9) -0.0015(10) C39 0.0192(12) 0.0180(12) 0.0188(12) -0.0008(9) -0.0005(9) -0.0011(10) C40 0.0192(12) 0.0180(12) 0.0181(12) -0.0019(9) -0.0004(9) -0.0014(9) C41 0.0177(12) 0.0195(12) 0.0191(12) -0.0012(10) 0.0024(9) -0.0005(10) C42 0.0200(12) 0.0215(13) 0.0180(12) 0.0004(10) 0.0005(9) -0.0039(10) C43 0.0289(14) 0.0190(13) 0.0216(13) 0.0019(10) -0.0036(10) -0.0018(10) C44 0.0364(16) 0.0257(14) 0.0266(14) 0.0034(11) -0.0007(12) -0.0095(12) C45 0.0414(17) 0.0230(14) 0.0363(16) 0.0098(12) -0.0115(13) -0.0095(13) C46 0.0356(16) 0.0195(14) 0.0473(18) 0.0015(12) -0.0184(14) -0.0009(12) C47 0.0234(14) 0.0213(13) 0.0417(16) -0.0001(12) -0.0090(12) -0.0001(11) C48 0.0230(13) 0.0215(13) 0.0243(13) 0.0019(10) -0.0059(10) -0.0040(10) C49 0.0232(13) 0.0150(12) 0.0199(12) -0.0004(9) 0.0037(10) 0.0011(10) C50 0.0264(14) 0.0217(13) 0.0311(15) -0.0014(11) -0.0049(11) -0.0022(11) C51 0.0275(15) 0.0266(14) 0.0359(16) -0.0010(12) -0.0083(12) 0.0049(12) C52 0.0359(16) 0.0187(13) 0.0308(15) 0.0014(11) 0.0000(12) 0.0090(11) C53 0.0347(15) 0.0170(13) 0.0291(14) -0.0016(11) 0.0022(12) -0.0018(11) C54 0.0240(13) 0.0239(13) 0.0214(13) -0.0021(10) 0.0001(10) -0.0027(10) C55 0.0198(12) 0.0162(12) 0.0215(12) 0.0033(9) 0.0005(10) 0.0008(9) C56 0.0238(14) 0.0321(15) 0.0257(14) -0.0071(11) 0.0033(11) -0.0013(11) C57 0.0197(13) 0.0371(16) 0.0364(16) -0.0083(13) 0.0002(11) -0.0042(12) C58 0.0211(13) 0.0286(14) 0.0313(15) -0.0051(12) 0.0072(11) 0.0000(11) C59 0.0265(14) 0.0381(16) 0.0240(14) -0.0074(12) 0.0024(11) 0.0017(12) C60 0.0182(13) 0.0319(15) 0.0254(13) -0.0031(11) -0.0013(10) 0.0004(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S1 C6 1.732(2) . ? S1 C7 1.750(2) . ? S2 C13 1.736(3) . ? S2 C12 1.751(2) . ? N1 C7 1.306(3) . ? N1 C1 1.388(3) . ? N2 C8 1.360(3) . ? N2 C11 1.366(3) . ? N3 C12 1.306(3) . ? N3 C18 1.388(3) . ? C1 C2 1.398(3) . ? C1 C6 1.401(3) . ? C2 C3 1.387(4) . ? C3 C4 1.398(4) . ? C4 C5 1.378(4) . ? C5 C6 1.398(3) . ? C7 C8 1.449(3) . ? C8 C9 1.390(3) . ? C9 C10 1.419(3) . ? C9 C19 1.489(3) . ? C10 C11 1.391(3) . ? C10 C25 1.484(3) . ? C11 C12 1.450(3) . ? C13 C14 1.397(4) . ? C13 C18 1.404(3) . ? C14 C15 1.379(4) . ? C15 C16 1.397(4) . ? C16 C17 1.380(4) . ? C17 C18 1.400(4) . ? C19 C24 1.388(4) . ? C19 C20 1.388(4) . ? C20 C21 1.387(4) . ? C21 C22 1.382(4) . ? C22 C23 1.382(4) . ? C23 C24 1.391(4) . ? C25 C30 1.391(3) . ? C25 C26 1.402(4) . ? C26 C27 1.390(4) . ? C27 C28 1.382(4) . ? C28 C29 1.386(4) . ? C29 C30 1.390(4) . ? S3 C36 1.738(2) . ? S3 C37 1.752(3) . ? S4 C43 1.735(3) . ? S4 C42 1.756(2) . ? N4 C37 1.308(3) . ? N4 C31 1.390(3) . ? N5 C41 1.370(3) . ? N5 C38 1.374(3) . ? N6 C42 1.303(3) . ? N6 C48 1.390(3) . ? C31 C32 1.399(3) . ? C31 C36 1.404(3) . ? C32 C33 1.385(4) . ? C33 C34 1.399(4) . ? C34 C35 1.380(4) . ? C35 C36 1.392(3) . ? C37 C38 1.443(3) . ? C38 C39 1.394(3) . ? C39 C40 1.422(3) . ? C39 C49 1.485(3) . ? C40 C41 1.383(3) . ? C40 C55 1.485(3) . ? C41 C42 1.443(3) . ? C43 C44 1.399(4) . ? C43 C48 1.401(4) . ? C44 C45 1.377(4) . ? C45 C46 1.398(4) . ? C46 C47 1.380(4) . ? C47 C48 1.399(4) . ? C49 C54 1.389(3) . ? C49 C50 1.395(4) . ? C50 C51 1.388(4) . ? C51 C52 1.384(4) . ? C52 C53 1.380(4) . ? C53 C54 1.389(4) . ? C55 C56 1.387(4) . ? C55 C60 1.390(4) . ? C56 C57 1.385(4) . ? C57 C58 1.388(4) . ? C58 C59 1.373(4) . ? C59 C60 1.387(4) . ? 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 C6 S1 C7 88.69(12) . . ? C13 S2 C12 88.79(12) . . ? C7 N1 C1 110.2(2) . . ? C8 N2 C11 110.0(2) . . ? C12 N3 C18 110.3(2) . . ? N1 C1 C2 125.0(2) . . ? N1 C1 C6 115.2(2) . . ? C2 C1 C6 119.9(2) . . ? C3 C2 C1 118.5(2) . . ? C2 C3 C4 121.1(2) . . ? C5 C4 C3 121.0(2) . . ? C4 C5 C6 118.2(2) . . ? C5 C6 C1 121.3(2) . . ? C5 C6 S1 128.8(2) . . ? C1 C6 S1 109.83(18) . . ? N1 C7 C8 121.3(2) . . ? N1 C7 S1 116.16(18) . . ? C8 C7 S1 122.56(18) . . ? N2 C8 C9 108.1(2) . . ? N2 C8 C7 118.5(2) . . ? C9 C8 C7 133.4(2) . . ? C8 C9 C10 107.1(2) . . ? C8 C9 C19 126.0(2) . . ? C10 C9 C19 126.9(2) . . ? C11 C10 C9 106.9(2) . . ? C11 C10 C25 127.4(2) . . ? C9 C10 C25 125.7(2) . . ? N2 C11 C10 107.9(2) . . ? N2 C11 C12 117.9(2) . . ? C10 C11 C12 133.8(2) . . ? N3 C12 C11 121.0(2) . . ? N3 C12 S2 116.14(19) . . ? C11 C12 S2 122.81(19) . . ? C14 C13 C18 121.3(2) . . ? C14 C13 S2 129.2(2) . . ? C18 C13 S2 109.56(19) . . ? C15 C14 C13 118.2(2) . . ? C14 C15 C16 121.0(2) . . ? C17 C16 C15 121.2(3) . . ? C16 C17 C18 118.7(2) . . ? N3 C18 C17 125.1(2) . . ? N3 C18 C13 115.2(2) . . ? C17 C18 C13 119.6(2) . . ? C24 C19 C20 118.8(2) . . ? C24 C19 C9 120.0(2) . . ? C20 C19 C9 121.2(2) . . ? C21 C20 C19 120.7(2) . . ? C22 C21 C20 120.3(3) . . ? C21 C22 C23 119.4(3) . . ? C22 C23 C24 120.4(3) . . ? C19 C24 C23 120.3(3) . . ? C30 C25 C26 119.2(2) . . ? C30 C25 C10 120.7(2) . . ? C26 C25 C10 120.1(2) . . ? C27 C26 C25 119.8(2) . . ? C28 C27 C26 120.6(3) . . ? C27 C28 C29 119.9(2) . . ? C28 C29 C30 120.1(2) . . ? C29 C30 C25 120.4(3) . . ? C36 S3 C37 88.97(12) . . ? C43 S4 C42 88.48(12) . . ? C37 N4 C31 110.4(2) . . ? C41 N5 C38 109.8(2) . . ? C42 N6 C48 110.2(2) . . ? N4 C31 C32 125.5(2) . . ? N4 C31 C36 115.3(2) . . ? C32 C31 C36 119.2(2) . . ? C33 C32 C31 118.6(2) . . ? C32 C33 C34 121.2(2) . . ? C35 C34 C33 121.1(2) . . ? C34 C35 C36 117.5(2) . . ? C35 C36 C31 122.3(2) . . ? C35 C36 S3 128.2(2) . . ? C31 C36 S3 109.45(18) . . ? N4 C37 C38 121.9(2) . . ? N4 C37 S3 115.89(18) . . ? C38 C37 S3 122.19(19) . . ? N5 C38 C39 107.8(2) . . ? N5 C38 C37 117.9(2) . . ? C39 C38 C37 134.3(2) . . ? C38 C39 C40 106.8(2) . . ? C38 C39 C49 129.0(2) . . ? C40 C39 C49 124.2(2) . . ? C41 C40 C39 107.7(2) . . ? C41 C40 C55 126.1(2) . . ? C39 C40 C55 126.0(2) . . ? N5 C41 C40 107.9(2) . . ? N5 C41 C42 119.2(2) . . ? C40 C41 C42 132.8(2) . . ? N6 C42 C41 122.1(2) . . ? N6 C42 S4 116.24(18) . . ? C41 C42 S4 121.62(19) . . ? C44 C43 C48 121.4(2) . . ? C44 C43 S4 128.7(2) . . ? C48 C43 S4 109.90(18) . . ? C45 C44 C43 117.8(3) . . ? C44 C45 C46 121.3(3) . . ? C47 C46 C45 121.3(3) . . ? C46 C47 C48 118.3(3) . . ? N6 C48 C47 124.9(2) . . ? N6 C48 C43 115.1(2) . . ? C47 C48 C43 120.0(2) . . ? C54 C49 C50 118.5(2) . . ? C54 C49 C39 123.2(2) . . ? C50 C49 C39 118.3(2) . . ? C51 C50 C49 120.5(2) . . ? C52 C51 C50 120.2(3) . . ? C53 C52 C51 119.9(2) . . ? C52 C53 C54 119.9(3) . . ? C49 C54 C53 121.0(2) . . ? C56 C55 C60 119.0(2) . . ? C56 C55 C40 122.0(2) . . ? C60 C55 C40 119.0(2) . . ? C57 C56 C55 120.3(3) . . ? C56 C57 C58 120.3(3) . . ? C59 C58 C57 119.5(2) . . ? C58 C59 C60 120.5(3) . . ? C59 C60 C55 120.3(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.318 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.071 _iucr_refine_instruction_details ; TITL 2010acc1015 in P-1 CELL 0.71069 9.9600 13.5973 17.4476 89.652 87.180 86.996 ZERR 4.00 0.0002 0.0003 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H N S UNIT 120 76 12 8 MERG 2 SHEL 7 0.77 FMAP 2 HTAB PLAN 25 SIZE 0.03 0.18 0.22 ACTA 55.00 LIST 1 L.S. 4 TEMP -153.00 WGHT 0.000000 4.253500 FVAR 0.33725 MOLE 1 S1 4 0.123628 0.735243 0.581198 11.00000 0.02327 0.01631 = 0.02198 -0.00070 0.00359 0.00079 S2 4 0.412961 0.208206 0.462924 11.00000 0.02213 0.01553 = 0.02786 -0.00059 0.00140 0.00057 N1 3 0.293752 0.705197 0.464429 11.00000 0.01945 0.01690 = 0.02391 -0.00041 -0.00030 0.00035 N2 3 0.327412 0.502073 0.479413 11.00000 0.02346 0.01568 = 0.02236 -0.00056 0.00306 -0.00020 H902 2 0.373952 0.528287 0.442076 11.00000 0.02691 N3 3 0.470877 0.366434 0.385832 11.00000 0.02180 0.01736 = 0.02738 0.00109 -0.00085 0.00206 C1 1 0.265081 0.806077 0.468773 11.00000 0.01951 0.01766 = 0.01990 -0.00147 -0.00298 0.00020 C2 1 0.319249 0.875815 0.418609 11.00000 0.02302 0.02214 = 0.02377 -0.00026 0.00054 -0.00114 AFIX 43 H2 2 0.381481 0.856178 0.377863 11.00000 -1.20000 AFIX 0 C3 1 0.280157 0.974301 0.429620 11.00000 0.02584 0.01868 = 0.03096 0.00275 -0.00108 -0.00410 AFIX 43 H3 2 0.314501 1.022342 0.395214 11.00000 -1.20000 AFIX 0 C4 1 0.191081 1.004084 0.490481 11.00000 0.02477 0.01583 = 0.03814 -0.00065 -0.00318 -0.00022 AFIX 43 H4 2 0.167153 1.072120 0.497372 11.00000 -1.20000 AFIX 0 C5 1 0.137465 0.936200 0.540633 11.00000 0.02494 0.01911 = 0.02933 -0.00348 0.00056 0.00032 AFIX 43 H5 2 0.076676 0.956486 0.581875 11.00000 -1.20000 AFIX 0 C6 1 0.174974 0.836643 0.529165 11.00000 0.01862 0.01770 = 0.02024 0.00011 -0.00334 -0.00296 C7 1 0.226717 0.660108 0.519157 11.00000 0.01933 0.01798 = 0.01890 -0.00188 -0.00150 0.00164 C8 1 0.239588 0.554042 0.527885 11.00000 0.01818 0.01906 = 0.02136 -0.00047 -0.00142 -0.00053 C9 1 0.181589 0.488170 0.579275 11.00000 0.01856 0.01688 = 0.02390 -0.00037 -0.00399 -0.00024 C10 1 0.239254 0.393121 0.560837 11.00000 0.01847 0.01704 = 0.02270 -0.00039 -0.00348 -0.00027 C11 1 0.328187 0.404259 0.497731 11.00000 0.02118 0.01414 = 0.02589 -0.00099 -0.00398 -0.00022 C12 1 0.405821 0.335735 0.447501 11.00000 0.01832 0.01724 = 0.02449 0.00012 -0.00361 -0.00031 C13 1 0.513727 0.194390 0.379241 11.00000 0.01665 0.02061 = 0.02652 -0.00106 -0.00326 0.00074 C14 1 0.570875 0.108347 0.345233 11.00000 0.02061 0.01940 = 0.03352 -0.00227 -0.00412 0.00104 AFIX 43 H14 2 0.559698 0.045957 0.368814 11.00000 -1.20000 AFIX 0 C15 1 0.643962 0.116418 0.276496 11.00000 0.02015 0.02576 = 0.03146 -0.00797 -0.00250 0.00618 AFIX 43 H15 2 0.682937 0.058716 0.252157 11.00000 -1.20000 AFIX 0 C16 1 0.661534 0.208196 0.242126 11.00000 0.02524 0.03131 = 0.02560 -0.00086 0.00097 0.00420 AFIX 43 H16 2 0.711389 0.211781 0.194443 11.00000 -1.20000 AFIX 0 C17 1 0.607824 0.293733 0.276149 11.00000 0.02556 0.02512 = 0.02923 0.00360 -0.00218 0.00232 AFIX 43 H17 2 0.621803 0.355938 0.252862 11.00000 -1.20000 AFIX 0 C18 1 0.532322 0.287115 0.345654 11.00000 0.01918 0.02030 = 0.02431 -0.00183 -0.00505 0.00048 C19 1 0.081451 0.514018 0.643111 11.00000 0.02357 0.01378 = 0.02372 0.00050 0.00078 -0.00177 C20 1 -0.048941 0.547537 0.628634 11.00000 0.02251 0.02388 = 0.02455 0.00167 0.00076 -0.00128 AFIX 43 H20 2 -0.076433 0.551111 0.577277 11.00000 -1.20000 AFIX 0 C21 1 -0.139503 0.575863 0.688346 11.00000 0.02132 0.02765 = 0.03749 0.00728 0.00528 0.00121 AFIX 43 H21 2 -0.228263 0.599087 0.677632 11.00000 -1.20000 AFIX 0 C22 1 -0.101165 0.570445 0.763346 11.00000 0.03569 0.03163 = 0.03059 0.00104 0.01260 -0.00210 AFIX 43 H22 2 -0.162583 0.591123 0.804185 11.00000 -1.20000 AFIX 0 C23 1 0.027357 0.534669 0.778439 11.00000 0.04264 0.04033 = 0.01970 0.00139 0.00117 -0.00205 AFIX 43 H23 2 0.053690 0.529511 0.829968 11.00000 -1.20000 AFIX 0 C24 1 0.118384 0.506170 0.718647 11.00000 0.02515 0.03149 = 0.02696 0.00119 -0.00370 0.00064 AFIX 43 H24 2 0.206277 0.481209 0.729588 11.00000 -1.20000 AFIX 0 C25 1 0.207081 0.300187 0.601115 11.00000 0.02408 0.01615 = 0.02039 -0.00097 -0.00083 0.00024 C26 1 0.075492 0.268046 0.603212 11.00000 0.02587 0.02273 = 0.02762 0.00162 -0.00641 0.00109 AFIX 43 H26 2 0.006780 0.305415 0.578493 11.00000 -1.20000 AFIX 0 C27 1 0.045831 0.181338 0.641563 11.00000 0.02656 0.02665 = 0.03162 0.00130 0.00113 -0.00734 AFIX 43 H27 2 -0.043326 0.159538 0.642783 11.00000 -1.20000 AFIX 0 C28 1 0.144903 0.126586 0.677924 11.00000 0.04083 0.01744 = 0.02129 -0.00001 -0.00077 -0.00346 AFIX 43 H28 2 0.123981 0.067153 0.703681 11.00000 -1.20000 AFIX 0 C29 1 0.274880 0.158553 0.676742 11.00000 0.03616 0.01968 = 0.02082 0.00163 -0.00504 0.00432 AFIX 43 H29 2 0.342958 0.121176 0.701981 11.00000 -1.20000 AFIX 0 C30 1 0.305766 0.245202 0.638692 11.00000 0.02605 0.02159 = 0.02281 -0.00234 -0.00396 0.00185 AFIX 43 H30 2 0.394857 0.267022 0.638343 11.00000 -1.20000 AFIX 0 MOLE 2 S3 4 0.682477 0.279204 -0.038789 11.00000 0.01958 0.01893 = 0.02482 0.00336 0.00207 -0.00048 S4 4 0.319219 -0.111885 0.214156 11.00000 0.02503 0.02041 = 0.02547 0.00271 0.00639 -0.00071 N4 3 0.804258 0.113096 -0.000915 11.00000 0.01842 0.02173 = 0.02028 -0.00046 0.00168 -0.00190 N5 3 0.588154 0.035062 0.081370 11.00000 0.02085 0.01773 = 0.02153 0.00053 0.00288 0.00096 H905 2 0.650932 -0.006517 0.067985 11.00000 0.03911 N6 3 0.552875 -0.152894 0.144333 11.00000 0.01809 0.01994 = 0.02523 0.00096 -0.00224 -0.00068 C31 1 0.892928 0.161240 -0.050362 11.00000 0.01825 0.02060 = 0.01925 -0.00047 -0.00187 -0.00413 C32 1 1.021381 0.124549 -0.075376 11.00000 0.01991 0.02746 = 0.02506 -0.00139 -0.00164 0.00144 AFIX 43 H32 2 1.057808 0.063867 -0.056125 11.00000 -1.20000 AFIX 0 C33 1 1.094280 0.178605 -0.128809 11.00000 0.01751 0.03589 = 0.02553 -0.00198 0.00161 -0.00449 AFIX 43 H33 2 1.181486 0.154356 -0.146418 11.00000 -1.20000 AFIX 0 C34 1 1.041935 0.268246 -0.157346 11.00000 0.02425 0.03178 = 0.02475 0.00194 0.00386 -0.00962 AFIX 43 H34 2 1.093336 0.303031 -0.194843 11.00000 -1.20000 AFIX 0 C35 1 0.916901 0.307013 -0.131958 11.00000 0.02283 0.02470 = 0.02467 0.00268 -0.00043 -0.00518 AFIX 43 H35 2 0.881914 0.368464 -0.150582 11.00000 -1.20000 AFIX 0 C36 1 0.843967 0.252746 -0.078061 11.00000 0.01873 0.01933 = 0.02197 -0.00203 0.00069 -0.00255 C37 1 0.690998 0.165667 0.009193 11.00000 0.01999 0.02012 = 0.01789 -0.00173 -0.00157 -0.00222 C38 1 0.578330 0.130273 0.054612 11.00000 0.01934 0.01858 = 0.01732 0.00080 -0.00075 -0.00155 C39 1 0.452622 0.171482 0.079370 11.00000 0.01924 0.01798 = 0.01875 -0.00076 -0.00045 -0.00111 C40 1 0.386742 0.097651 0.122697 11.00000 0.01918 0.01798 = 0.01814 -0.00188 -0.00036 -0.00136 C41 1 0.472256 0.014187 0.122421 11.00000 0.01768 0.01948 = 0.01909 -0.00115 0.00236 -0.00050 C42 1 0.460253 -0.082554 0.155734 11.00000 0.02002 0.02150 = 0.01802 0.00039 0.00055 -0.00392 C43 1 0.391400 -0.229976 0.223777 11.00000 0.02890 0.01903 = 0.02157 0.00191 -0.00357 -0.00180 C44 1 0.339657 -0.310393 0.263530 11.00000 0.03640 0.02570 = 0.02662 0.00339 -0.00070 -0.00945 AFIX 43 H44 2 0.255882 -0.304378 0.292017 11.00000 -1.20000 AFIX 0 C45 1 0.414225 -0.398531 0.259975 11.00000 0.04136 0.02297 = 0.03633 0.00978 -0.01146 -0.00949 AFIX 43 H45 2 0.382282 -0.453846 0.287454 11.00000 -1.20000 AFIX 0 C46 1 0.536053 -0.408195 0.216703 11.00000 0.03558 0.01946 = 0.04727 0.00148 -0.01844 -0.00087 AFIX 43 H46 2 0.583906 -0.470476 0.214030 11.00000 -1.20000 AFIX 0 C47 1 0.588171 -0.328991 0.177780 11.00000 0.02343 0.02133 = 0.04173 -0.00010 -0.00904 -0.00007 AFIX 43 H47 2 0.671543 -0.335882 0.148960 11.00000 -1.20000 AFIX 0 C48 1 0.515057 -0.238286 0.181861 11.00000 0.02304 0.02148 = 0.02432 0.00188 -0.00595 -0.00398 C49 1 0.391256 0.270957 0.063473 11.00000 0.02316 0.01497 = 0.01988 -0.00041 0.00368 0.00113 C50 1 0.269455 0.277588 0.027130 11.00000 0.02636 0.02171 = 0.03114 -0.00136 -0.00487 -0.00217 AFIX 43 H50 2 0.228999 0.219224 0.012591 11.00000 -1.20000 AFIX 0 C51 1 0.206903 0.368764 0.012041 11.00000 0.02750 0.02664 = 0.03589 -0.00103 -0.00832 0.00485 AFIX 43 H51 2 0.123493 0.372527 -0.012259 11.00000 -1.20000 AFIX 0 C52 1 0.265738 0.454247 0.032310 11.00000 0.03593 0.01872 = 0.03085 0.00142 0.00001 0.00899 AFIX 43 H52 2 0.223333 0.516608 0.021336 11.00000 -1.20000 AFIX 0 C53 1 0.386022 0.448774 0.068465 11.00000 0.03465 0.01703 = 0.02911 -0.00157 0.00217 -0.00185 AFIX 43 H53 2 0.426712 0.507347 0.082288 11.00000 -1.20000 AFIX 0 C54 1 0.447522 0.357459 0.084618 11.00000 0.02396 0.02394 = 0.02135 -0.00210 0.00006 -0.00265 AFIX 43 H54 2 0.529332 0.354132 0.110529 11.00000 -1.20000 AFIX 0 C55 1 0.255543 0.110912 0.166587 11.00000 0.01982 0.01618 = 0.02146 0.00327 0.00054 0.00077 C56 1 0.136272 0.083524 0.137083 11.00000 0.02384 0.03213 = 0.02568 -0.00708 0.00334 -0.00130 AFIX 43 H56 2 0.137142 0.055544 0.087290 11.00000 -1.20000 AFIX 0 C57 1 0.015894 0.096784 0.179891 11.00000 0.01965 0.03714 = 0.03635 -0.00827 0.00021 -0.00419 AFIX 43 H57 2 -0.065556 0.078590 0.159064 11.00000 -1.20000 AFIX 0 C58 1 0.013669 0.136513 0.253048 11.00000 0.02113 0.02863 = 0.03132 -0.00515 0.00720 0.00004 AFIX 43 H58 2 -0.068872 0.145129 0.282487 11.00000 -1.20000 AFIX 0 C59 1 0.131639 0.163270 0.282559 11.00000 0.02654 0.03812 = 0.02399 -0.00737 0.00239 0.00172 AFIX 43 H59 2 0.130616 0.190075 0.332753 11.00000 -1.20000 AFIX 0 C60 1 0.252298 0.151459 0.239643 11.00000 0.01822 0.03194 = 0.02541 -0.00312 -0.00131 0.00037 AFIX 43 H60 2 0.333156 0.171182 0.260281 11.00000 -1.20000 HKLF 4 REM 2010acc1015 in P-1 REM R1 = 0.0591 for 8548 Fo > 4sig(Fo) and 0.0813 for all 10759 data REM 639 parameters refined using 0 restraints END WGHT 0.0000 4.2411 REM Highest difference peak 0.318, deepest hole -0.349, 1-sigma level 0.071 Q1 1 -0.2966 0.5462 0.7317 11.00000 0.05 0.32 Q2 1 0.4270 0.1406 0.1061 11.00000 0.05 0.29 Q3 1 0.2281 0.9835 0.4581 11.00000 0.05 0.29 Q4 1 0.3196 0.2747 0.0552 11.00000 0.05 0.28 Q5 1 0.1406 0.0935 0.0780 11.00000 0.05 0.28 Q6 1 0.1491 0.7998 0.5540 11.00000 0.05 0.28 Q7 1 0.7528 0.0619 0.2671 11.00000 0.05 0.28 Q8 1 0.0834 0.5641 0.8223 11.00000 0.05 0.27 Q9 1 0.3782 -0.2442 0.2649 11.00000 0.05 0.27 Q10 1 0.2373 0.1617 0.1927 11.00000 0.05 0.27 Q11 1 0.2035 0.5599 0.0238 11.00000 0.05 0.27 Q12 1 0.2798 0.9240 0.4181 11.00000 0.05 0.27 Q13 1 0.2597 0.2596 0.6025 11.00000 0.05 0.27 Q14 1 0.0776 0.5555 0.7519 11.00000 0.05 0.27 Q15 1 0.1275 0.8839 0.5130 11.00000 0.05 0.27 Q16 1 0.3977 0.3135 0.0832 11.00000 0.05 0.27 Q17 1 0.4171 0.2203 0.0755 11.00000 0.05 0.27 Q18 1 0.4699 -0.2311 0.2184 11.00000 0.05 0.26 Q19 1 0.4511 -0.4089 0.2232 11.00000 0.05 0.26 Q20 1 0.6709 -0.4620 0.1206 11.00000 0.05 0.26 Q21 1 0.6195 -0.1221 0.1012 11.00000 0.05 0.26 Q22 1 0.4027 -0.0899 0.1841 11.00000 0.05 0.26 Q23 1 0.6625 0.2044 0.2038 11.00000 0.05 0.26 Q24 1 0.2376 0.8274 0.5102 11.00000 0.05 0.26 Q25 1 0.0636 0.4618 0.0120 11.00000 0.05 0.26 ; #===END data_2010acc1121_trimer_886 _database_code_depnum_ccdc_archive 'CCDC 817764' #TrackingRef '- Ogden_Dalton_combined.cif.txt' _chemical_compound_source 'Massimiliano Massi' _database_code_CSD 10AC1121 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H56 Cl3 Cu3 N9 S6, 1.4(C H Cl3), 0.6(O)' _chemical_formula_sum 'C91.40 H57.40 Cl7.20 Cu3 N9 O0.60 S6' _chemical_formula_weight 1929.48 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' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 '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 13.4166(9) _cell_length_b 15.8954(10) _cell_length_c 19.7847(13) _cell_angle_alpha 96.701(4) _cell_angle_beta 95.457(4) _cell_angle_gamma 95.884(4) _cell_volume 4143.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 166404 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1958 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8692 _exptl_absorpt_correction_T_max 0.9764 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56588 _diffrn_reflns_av_R_equivalents 0.1338 _diffrn_reflns_av_sigmaI/netI 0.1582 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.02 _reflns_number_total 14445 _reflns_number_gt 8265 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Images generated using CrystalMaker: a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd, Oxford, England (www.crystalmaker.com) ; _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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 an area of mixed CHCl3 and H2O solvent that has been modelled as a partially occupied mixture of the two species. Thermal parameter restraints and constraints were used for the solvent, and mild thermal parameter restraints applied to the remainder of the structure. Hydrogen atoms were not located for the water, and the remainder were placed in calculated positions and refined 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^)+(0.0000P)^2^+121.4550P] 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 14445 _refine_ls_number_parameters 1084 _refine_ls_number_restraints 989 _refine_ls_R_factor_all 0.2480 _refine_ls_R_factor_gt 0.1559 _refine_ls_wR_factor_ref 0.3124 _refine_ls_wR_factor_gt 0.2671 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.054 _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 Cu1 Cu 0.32545(13) 0.46615(10) 0.36353(9) 0.0340(4) Uani 1 1 d . . . Cl1 Cl 0.3823(3) 0.5909(2) 0.33685(18) 0.0392(9) Uani 1 1 d . . . S1 S -0.0163(3) 0.4046(2) 0.37406(19) 0.0387(9) Uani 1 1 d U . . S2 S 0.5328(3) 0.3144(2) 0.48637(18) 0.0350(8) Uani 1 1 d U . . N1 N 0.1604(9) 0.4703(7) 0.3505(6) 0.037(2) Uani 1 1 d U . . N2 N 0.2720(9) 0.3689(7) 0.4013(6) 0.034(2) Uani 1 1 d U . . N3 N 0.4573(9) 0.4241(6) 0.4159(5) 0.031(2) Uani 1 1 d U . . C1 C -0.0086(11) 0.4964(9) 0.3316(7) 0.040(3) Uani 1 1 d U . . C2 C -0.0873(12) 0.5398(9) 0.3100(8) 0.046(3) Uani 1 1 d U . . H2 H -0.1538 0.5221 0.3160 0.055 Uiso 1 1 calc R . . C3 C -0.0613(12) 0.6113(10) 0.2790(8) 0.049(3) Uani 1 1 d U . . H3 H -0.1116 0.6427 0.2635 0.059 Uiso 1 1 calc R . . C4 C 0.0395(12) 0.6373(10) 0.2705(8) 0.051(3) Uani 1 1 d U . . H4 H 0.0550 0.6855 0.2493 0.061 Uiso 1 1 calc R . . C5 C 0.1152(12) 0.5926(9) 0.2932(8) 0.046(3) Uani 1 1 d U . . H5 H 0.1820 0.6105 0.2882 0.056 Uiso 1 1 calc R . . C6 C 0.0908(11) 0.5203(9) 0.3237(8) 0.041(2) Uani 1 1 d U . . C7 C 0.1126(11) 0.4076(9) 0.3765(7) 0.036(2) Uani 1 1 d U . . C8 C 0.1726(11) 0.3493(8) 0.4080(7) 0.035(2) Uani 1 1 d U . . C9 C 0.1638(11) 0.2846(8) 0.4505(7) 0.035(2) Uani 1 1 d U . . C10 C 0.2638(11) 0.2686(8) 0.4723(7) 0.034(2) Uani 1 1 d U . . C11 C 0.3287(10) 0.3235(8) 0.4413(7) 0.032(2) Uani 1 1 d U . . C12 C 0.4324(10) 0.3550(8) 0.4441(6) 0.030(2) Uani 1 1 d U . . C13 C 0.6144(11) 0.3964(8) 0.4663(7) 0.036(2) Uani 1 1 d U . . C14 C 0.7173(11) 0.4136(9) 0.4834(7) 0.039(3) Uani 1 1 d U . . H14 H 0.7526 0.3785 0.5090 0.047 Uiso 1 1 calc R . . C15 C 0.7667(12) 0.4852(9) 0.4610(7) 0.040(3) Uani 1 1 d U . . H15 H 0.8359 0.4985 0.4717 0.048 Uiso 1 1 calc R . . C16 C 0.7128(11) 0.5368(9) 0.4227(7) 0.040(3) Uani 1 1 d U . . H16 H 0.7472 0.5846 0.4090 0.049 Uiso 1 1 calc R . . C17 C 0.6108(11) 0.5200(8) 0.4045(7) 0.038(2) Uani 1 1 d U . . H17 H 0.5767 0.5548 0.3780 0.045 Uiso 1 1 calc R . . C18 C 0.5595(11) 0.4491(8) 0.4269(7) 0.035(2) Uani 1 1 d U . . C19 C 0.0629(11) 0.2515(8) 0.4722(7) 0.036(2) Uani 1 1 d U . . C20 C 0.0138(11) 0.1743(9) 0.4407(7) 0.038(3) Uani 1 1 d U . . H20 H 0.0439 0.1425 0.4076 0.045 Uiso 1 1 calc R . . C21 C -0.0795(11) 0.1438(10) 0.4578(8) 0.045(3) Uani 1 1 d U . . H21 H -0.1132 0.0927 0.4353 0.054 Uiso 1 1 calc R . . C22 C -0.1217(12) 0.1898(9) 0.5082(8) 0.044(3) Uani 1 1 d U . . H22 H -0.1833 0.1688 0.5211 0.053 Uiso 1 1 calc R . . C23 C -0.0749(11) 0.2646(9) 0.5389(8) 0.043(3) Uani 1 1 d U . . H23 H -0.1057 0.2957 0.5722 0.051 Uiso 1 1 calc R . . C24 C 0.0191(11) 0.2976(9) 0.5223(7) 0.042(3) Uani 1 1 d U . . H24 H 0.0512 0.3494 0.5446 0.051 Uiso 1 1 calc R . . C25 C 0.2889(11) 0.2084(8) 0.5200(7) 0.037(2) Uani 1 1 d U . . C26 C 0.3608(11) 0.2308(9) 0.5760(7) 0.040(3) Uani 1 1 d U . . H26 H 0.3910 0.2869 0.5842 0.048 Uiso 1 1 calc R . . C27 C 0.3903(12) 0.1747(10) 0.6202(8) 0.046(3) Uani 1 1 d U . . H27 H 0.4406 0.1929 0.6562 0.056 Uiso 1 1 calc R . . C28 C 0.3460(11) 0.0937(9) 0.6112(8) 0.043(3) Uani 1 1 d U . . H28 H 0.3630 0.0566 0.6423 0.052 Uiso 1 1 calc R . . C29 C 0.2745(12) 0.0657(9) 0.5553(8) 0.045(3) Uani 1 1 d U . . H29 H 0.2452 0.0093 0.5484 0.054 Uiso 1 1 calc R . . C30 C 0.2464(11) 0.1222(8) 0.5094(8) 0.040(3) Uani 1 1 d U . . H30 H 0.1996 0.1028 0.4716 0.048 Uiso 1 1 calc R . . Cu2 Cu 0.28712(14) 0.26103(10) 0.26149(9) 0.0349(4) Uani 1 1 d . . . Cl2 Cl 0.3418(3) 0.3880(2) 0.23742(18) 0.0392(9) Uani 1 1 d . . . S3 S -0.0528(3) 0.1717(2) 0.24632(19) 0.0386(9) Uani 1 1 d U . . S4 S 0.5047(3) 0.0937(2) 0.3608(2) 0.0414(9) Uani 1 1 d U . . N4 N 0.1210(9) 0.2534(7) 0.2393(5) 0.032(2) Uani 1 1 d U . . N5 N 0.2382(9) 0.1635(6) 0.2984(5) 0.032(2) Uani 1 1 d U . . N6 N 0.4262(9) 0.2151(7) 0.3037(6) 0.036(2) Uani 1 1 d U . . C31 C -0.0474(12) 0.2652(9) 0.2088(7) 0.041(3) Uani 1 1 d U . . C32 C -0.1295(13) 0.3023(9) 0.1799(7) 0.047(3) Uani 1 1 d U . . H32 H -0.1959 0.2784 0.1791 0.057 Uiso 1 1 calc R . . C33 C -0.1036(13) 0.3784(9) 0.1524(8) 0.049(3) Uani 1 1 d U . . H33 H -0.1549 0.4052 0.1320 0.059 Uiso 1 1 calc R . . C34 C -0.0048(13) 0.4153(9) 0.1544(8) 0.049(3) Uani 1 1 d U . . H34 H 0.0078 0.4664 0.1364 0.059 Uiso 1 1 calc R . . C35 C 0.0759(12) 0.3776(8) 0.1826(7) 0.043(3) Uani 1 1 d U . . H35 H 0.1423 0.4013 0.1831 0.051 Uiso 1 1 calc R . . C36 C 0.0512(12) 0.3018(8) 0.2102(7) 0.039(2) Uani 1 1 d U . . C37 C 0.0789(10) 0.1835(8) 0.2595(6) 0.032(2) Uani 1 1 d U . . C38 C 0.1423(10) 0.1278(8) 0.2897(7) 0.031(2) Uani 1 1 d U . . C39 C 0.1368(10) 0.0450(8) 0.3108(6) 0.030(2) Uani 1 1 d U . . C40 C 0.2377(10) 0.0342(8) 0.3334(6) 0.031(2) Uani 1 1 d U . . C41 C 0.2991(10) 0.1086(8) 0.3236(7) 0.032(2) Uani 1 1 d U . . C42 C 0.4030(11) 0.1408(8) 0.3287(7) 0.036(2) Uani 1 1 d U . . C43 C 0.5861(11) 0.1788(9) 0.3417(8) 0.043(3) Uani 1 1 d U . . C44 C 0.6895(12) 0.1904(10) 0.3523(8) 0.050(3) Uani 1 1 d U . . H44 H 0.7253 0.1503 0.3715 0.060 Uiso 1 1 calc R . . C45 C 0.7382(13) 0.2629(10) 0.3337(8) 0.052(3) Uani 1 1 d U . . H45 H 0.8081 0.2733 0.3413 0.062 Uiso 1 1 calc R . . C46 C 0.6829(12) 0.3211(10) 0.3034(8) 0.052(3) Uani 1 1 d U . . H46 H 0.7174 0.3695 0.2907 0.062 Uiso 1 1 calc R . . C47 C 0.5798(12) 0.3094(9) 0.2918(8) 0.043(3) Uani 1 1 d U . . H47 H 0.5444 0.3488 0.2714 0.052 Uiso 1 1 calc R . . C48 C 0.5302(11) 0.2368(9) 0.3114(7) 0.040(2) Uani 1 1 d U . . C49 C 0.0451(11) -0.0154(8) 0.3122(7) 0.034(2) Uani 1 1 d U . . C50 C 0.0338(11) -0.0534(8) 0.3701(7) 0.037(2) Uani 1 1 d U . . H50 H 0.0817 -0.0396 0.4080 0.044 Uiso 1 1 calc R . . C51 C -0.0506(11) -0.1135(9) 0.3723(8) 0.041(3) Uani 1 1 d U . . H51 H -0.0601 -0.1378 0.4120 0.050 Uiso 1 1 calc R . . C52 C -0.1180(11) -0.1354(9) 0.3156(8) 0.044(3) Uani 1 1 d U . . H52 H -0.1733 -0.1754 0.3166 0.053 Uiso 1 1 calc R . . C53 C -0.1052(12) -0.0988(10) 0.2561(8) 0.047(3) Uani 1 1 d U . . H53 H -0.1503 -0.1151 0.2170 0.056 Uiso 1 1 calc R . . C54 C -0.0238(11) -0.0374(9) 0.2563(8) 0.040(3) Uani 1 1 d U . . H54 H -0.0161 -0.0107 0.2174 0.048 Uiso 1 1 calc R . . C55 C 0.2739(11) -0.0447(8) 0.3548(7) 0.033(2) Uani 1 1 d U . . C56 C 0.2405(11) -0.1245(8) 0.3182(7) 0.036(3) Uani 1 1 d U . . H56 H 0.1913 -0.1296 0.2810 0.043 Uiso 1 1 calc R . . C57 C 0.2802(11) -0.1960(8) 0.3369(7) 0.039(3) Uani 1 1 d U . . H57 H 0.2596 -0.2486 0.3111 0.047 Uiso 1 1 calc R . . C58 C 0.3497(11) -0.1907(9) 0.3931(7) 0.040(3) Uani 1 1 d U . . H58 H 0.3739 -0.2397 0.4064 0.048 Uiso 1 1 calc R . . C59 C 0.3830(11) -0.1129(9) 0.4295(7) 0.040(3) Uani 1 1 d U . . H59 H 0.4311 -0.1091 0.4671 0.048 Uiso 1 1 calc R . . C60 C 0.3467(10) -0.0403(8) 0.4113(7) 0.033(2) Uani 1 1 d U . . H60 H 0.3704 0.0122 0.4366 0.039 Uiso 1 1 calc R . . Cu3 Cu 0.23450(15) 0.04461(11) 0.13119(10) 0.0450(5) Uani 1 1 d . . . Cl3 Cl 0.3036(3) 0.1778(2) 0.13949(19) 0.0453(9) Uani 1 1 d . . . S5 S 0.0692(3) 0.0755(2) 0.1007(2) 0.0458(10) Uani 1 1 d U . . S6 S 0.4225(4) -0.1726(3) 0.1632(3) 0.0709(14) Uani 1 1 d U . . N7 N -0.0890(9) -0.0495(7) 0.0703(6) 0.041(2) Uani 1 1 d U . . H7 H -0.1065 -0.1032 0.0692 0.049 Uiso 1 1 calc R . . N8 N 0.1697(10) -0.0675(8) 0.1206(6) 0.046(2) Uani 1 1 d U . . N9 N 0.3610(9) -0.0226(7) 0.1570(5) 0.034(2) Uani 1 1 d U . . C61 C -0.2586(11) -0.0515(9) 0.0282(7) 0.042(3) Uani 1 1 d U . . H61 H -0.2607 -0.1106 0.0225 0.050 Uiso 1 1 calc R . . C62 C -0.3446(12) -0.0132(9) 0.0101(8) 0.047(3) Uani 1 1 d U . . H62 H -0.4047 -0.0468 -0.0065 0.056 Uiso 1 1 calc R . . C63 C -0.3407(12) 0.0723(10) 0.0165(8) 0.047(3) Uani 1 1 d U . . H63 H -0.3982 0.0973 0.0038 0.057 Uiso 1 1 calc R . . C64 C -0.2501(12) 0.1246(10) 0.0424(8) 0.047(3) Uani 1 1 d U . . H64 H -0.2473 0.1837 0.0466 0.057 Uiso 1 1 calc R . . C65 C -0.1669(12) 0.0864(9) 0.0612(7) 0.042(3) Uani 1 1 d U . . H65 H -0.1068 0.1197 0.0785 0.050 Uiso 1 1 calc R . . C66 C -0.1716(12) -0.0018(9) 0.0544(7) 0.043(2) Uani 1 1 d U . . C67 C 0.0118(12) -0.0261(9) 0.0869(7) 0.045(2) Uani 1 1 d U . . C68 C 0.0734(13) -0.0940(9) 0.0987(7) 0.044(2) Uani 1 1 d U . . C69 C 0.0604(12) -0.1846(9) 0.0881(7) 0.044(2) Uani 1 1 d U . . C70 C 0.1547(13) -0.2105(9) 0.1077(7) 0.046(2) Uani 1 1 d U . . C71 C 0.2225(13) -0.1349(10) 0.1280(7) 0.045(2) Uani 1 1 d U . . C72 C 0.3276(12) -0.1080(9) 0.1484(7) 0.044(2) Uani 1 1 d U . . C73 C 0.5123(14) -0.0847(12) 0.1786(9) 0.063(3) Uani 1 1 d U . . C74 C 0.6129(15) -0.0791(13) 0.1948(9) 0.069(3) Uani 1 1 d U . . H74 H 0.6442 -0.1278 0.2002 0.083 Uiso 1 1 calc R . . C75 C 0.6708(15) 0.0036(12) 0.2034(10) 0.072(3) Uani 1 1 d U . . H75 H 0.7400 0.0091 0.2158 0.086 Uiso 1 1 calc R . . C76 C 0.6214(14) 0.0770(13) 0.1929(9) 0.069(3) Uani 1 1 d U . . H76 H 0.6595 0.1300 0.1971 0.083 Uiso 1 1 calc R . . C77 C 0.5203(14) 0.0717(12) 0.1768(9) 0.064(3) Uani 1 1 d U . . H77 H 0.4901 0.1208 0.1707 0.077 Uiso 1 1 calc R . . C78 C 0.4597(13) -0.0087(11) 0.1691(9) 0.056(3) Uani 1 1 d U . . C79 C -0.0394(13) -0.2408(10) 0.0696(8) 0.049(3) Uani 1 1 d U . . C80 C -0.0865(13) -0.2534(10) 0.0017(8) 0.053(3) Uani 1 1 d U . . H80 H -0.0562 -0.2281 -0.0324 0.064 Uiso 1 1 calc R . . C81 C -0.1787(14) -0.3041(10) -0.0137(9) 0.056(3) Uani 1 1 d U . . H81 H -0.2108 -0.3117 -0.0582 0.068 Uiso 1 1 calc R . . C82 C -0.2214(14) -0.3421(11) 0.0352(9) 0.063(3) Uani 1 1 d U . . H82 H -0.2816 -0.3778 0.0246 0.076 Uiso 1 1 calc R . . C83 C -0.1764(15) -0.3282(12) 0.0989(10) 0.072(3) Uani 1 1 d U . . H83 H -0.2074 -0.3540 0.1326 0.086 Uiso 1 1 calc R . . C84 C -0.0854(14) -0.2770(11) 0.1179(9) 0.062(3) Uani 1 1 d U . . H84 H -0.0570 -0.2680 0.1633 0.075 Uiso 1 1 calc R . . C85 C 0.1788(13) -0.3015(10) 0.1027(8) 0.051(3) Uani 1 1 d U . . C86 C 0.1445(14) -0.3588(10) 0.0455(8) 0.057(3) Uani 1 1 d U . . H86 H 0.1047 -0.3415 0.0098 0.068 Uiso 1 1 calc R . . C87 C 0.1680(14) -0.4409(10) 0.0404(9) 0.060(3) Uani 1 1 d U . . H87 H 0.1452 -0.4785 0.0010 0.072 Uiso 1 1 calc R . . C88 C 0.2264(14) -0.4683(11) 0.0942(9) 0.060(3) Uani 1 1 d U . . H88 H 0.2401 -0.5247 0.0917 0.072 Uiso 1 1 calc R . . C89 C 0.2626(14) -0.4117(10) 0.1499(8) 0.055(3) Uani 1 1 d U . . H89 H 0.3047 -0.4284 0.1848 0.066 Uiso 1 1 calc R . . C90 C 0.2374(13) -0.3291(10) 0.1551(8) 0.054(3) Uani 1 1 d U . . H90 H 0.2602 -0.2917 0.1945 0.065 Uiso 1 1 calc R . . C91 C 0.5782(17) 0.5838(16) 0.2147(11) 0.052(4) Uani 0.70 1 d PU A 1 H91 H 0.5187 0.5654 0.2367 0.063 Uiso 0.70 1 calc PR A 1 Cl4 Cl 0.6515(5) 0.4983(4) 0.2026(3) 0.0590(16) Uani 0.70 1 d PU A 1 Cl5 Cl 0.5397(6) 0.6181(5) 0.1370(4) 0.083(2) Uani 0.70 1 d PU A 1 Cl6 Cl 0.6488(7) 0.6684(4) 0.2664(4) 0.087(2) Uani 0.70 1 d PU A 1 O2W O 0.493(3) 0.540(3) 0.117(2) 0.082(2) Uani 0.30 1 d PU B 2 C92 C 0.508(2) 0.6916(17) -0.0633(14) 0.080(2) Uani 0.70 1 d PU C 3 H92 H 0.5637 0.7050 -0.0899 0.096 Uiso 0.70 1 calc PR C 3 Cl7 Cl 0.5186(7) 0.5869(5) -0.0541(5) 0.096(3) Uani 0.70 1 d PU C 3 Cl8 Cl 0.4116(6) 0.7166(4) -0.1131(4) 0.081(2) Uani 0.70 1 d PU C 3 Cl9 Cl 0.5427(5) 0.7607(4) 0.0106(3) 0.0561(15) Uani 0.70 1 d P C 3 O1W O 0.363(3) 0.639(3) -0.015(2) 0.082(2) Uani 0.30 1 d P D 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 Cu1 0.0397(10) 0.0251(9) 0.0386(10) 0.0102(7) 0.0014(8) 0.0065(8) Cl1 0.049(2) 0.0238(17) 0.045(2) 0.0078(15) 0.0006(17) 0.0040(16) S1 0.038(2) 0.037(2) 0.044(2) 0.0108(16) 0.0064(17) 0.0086(17) S2 0.038(2) 0.0287(18) 0.040(2) 0.0118(15) 0.0009(16) 0.0066(15) N1 0.044(5) 0.030(5) 0.038(5) 0.000(4) 0.007(4) 0.013(4) N2 0.043(4) 0.025(5) 0.036(5) 0.009(4) 0.001(4) 0.009(4) N3 0.046(5) 0.020(4) 0.032(5) 0.002(4) 0.011(4) 0.013(4) C1 0.047(5) 0.034(5) 0.040(6) 0.010(5) 0.000(5) 0.009(4) C2 0.046(6) 0.042(6) 0.052(7) 0.011(5) 0.001(5) 0.014(5) C3 0.050(6) 0.044(6) 0.060(7) 0.019(5) -0.001(6) 0.023(5) C4 0.054(6) 0.043(6) 0.060(7) 0.023(5) -0.001(6) 0.010(5) C5 0.047(6) 0.036(6) 0.057(7) 0.015(5) -0.001(5) 0.007(5) C6 0.046(5) 0.034(5) 0.044(5) 0.010(4) 0.001(5) 0.010(4) C7 0.041(5) 0.033(5) 0.035(6) 0.003(4) 0.005(5) 0.010(4) C8 0.043(4) 0.029(5) 0.035(5) 0.005(4) 0.004(4) 0.008(4) C9 0.043(4) 0.027(5) 0.034(5) 0.006(4) 0.001(4) 0.002(4) C10 0.042(4) 0.026(4) 0.037(5) 0.007(4) 0.008(4) 0.009(4) C11 0.041(4) 0.025(5) 0.032(5) 0.005(4) 0.008(4) 0.010(4) C12 0.042(4) 0.023(5) 0.028(5) 0.005(4) 0.010(4) 0.012(4) C13 0.047(5) 0.027(5) 0.034(6) -0.002(4) 0.007(5) 0.007(4) C14 0.046(5) 0.032(5) 0.040(6) -0.004(5) 0.008(5) 0.010(5) C15 0.044(6) 0.035(6) 0.041(6) -0.005(5) 0.007(5) 0.010(4) C16 0.048(5) 0.035(6) 0.039(6) 0.001(5) 0.009(5) 0.008(5) C17 0.046(5) 0.029(5) 0.041(6) 0.005(4) 0.008(5) 0.012(5) C18 0.045(5) 0.024(4) 0.039(5) 0.001(4) 0.011(4) 0.011(4) C19 0.043(5) 0.030(5) 0.036(5) 0.010(4) 0.002(4) 0.004(4) C20 0.044(6) 0.034(5) 0.036(6) 0.008(5) 0.000(5) 0.004(5) C21 0.046(6) 0.042(6) 0.047(6) 0.008(5) 0.000(5) 0.002(5) C22 0.041(6) 0.045(6) 0.047(6) 0.015(5) 0.004(5) 0.006(5) C23 0.046(6) 0.040(6) 0.046(6) 0.013(5) 0.008(5) 0.009(5) C24 0.050(6) 0.036(6) 0.041(6) 0.010(5) 0.004(5) 0.005(5) C25 0.044(5) 0.030(4) 0.042(5) 0.013(4) 0.014(4) 0.011(4) C26 0.044(6) 0.038(5) 0.044(6) 0.023(5) 0.013(5) 0.011(5) C27 0.048(6) 0.047(6) 0.052(6) 0.025(5) 0.011(5) 0.013(5) C28 0.048(7) 0.041(5) 0.051(6) 0.023(5) 0.020(5) 0.019(5) C29 0.054(7) 0.035(5) 0.054(6) 0.020(5) 0.019(5) 0.007(5) C30 0.049(6) 0.031(5) 0.045(6) 0.011(5) 0.014(5) 0.011(5) Cu2 0.0474(11) 0.0241(9) 0.0351(10) 0.0076(7) 0.0040(8) 0.0087(8) Cl2 0.054(2) 0.0217(17) 0.042(2) 0.0049(14) 0.0042(17) 0.0039(16) S3 0.040(2) 0.039(2) 0.038(2) 0.0079(16) 0.0001(17) 0.0124(17) S4 0.039(2) 0.0320(19) 0.056(2) 0.0082(17) 0.0030(18) 0.0121(16) N4 0.047(5) 0.026(4) 0.026(5) 0.007(4) 0.003(4) 0.012(4) N5 0.046(4) 0.024(4) 0.029(5) 0.006(4) 0.006(4) 0.011(4) N6 0.042(5) 0.028(5) 0.039(5) 0.007(4) 0.003(4) 0.009(4) C31 0.057(5) 0.031(5) 0.036(6) 0.004(4) -0.002(5) 0.016(4) C32 0.062(6) 0.038(6) 0.042(6) 0.005(5) -0.004(5) 0.018(5) C33 0.062(6) 0.035(6) 0.050(6) 0.006(5) -0.008(6) 0.021(5) C34 0.066(6) 0.030(6) 0.052(7) 0.005(5) -0.005(6) 0.016(5) C35 0.058(6) 0.027(5) 0.045(6) 0.008(5) -0.003(5) 0.016(5) C36 0.055(5) 0.029(5) 0.034(5) 0.004(4) 0.001(5) 0.018(4) C37 0.043(5) 0.028(5) 0.026(5) 0.007(4) 0.003(5) 0.008(4) C38 0.043(4) 0.023(4) 0.028(5) 0.003(4) 0.008(4) 0.012(4) C39 0.044(4) 0.019(4) 0.029(5) -0.001(4) 0.012(4) 0.012(3) C40 0.045(4) 0.021(4) 0.028(5) 0.003(4) 0.008(4) 0.009(4) C41 0.042(4) 0.025(4) 0.030(5) 0.006(4) 0.007(4) 0.010(4) C42 0.043(4) 0.029(5) 0.036(6) 0.005(5) 0.002(5) 0.008(4) C43 0.043(5) 0.032(5) 0.051(6) -0.004(5) -0.002(5) 0.007(4) C44 0.042(5) 0.042(6) 0.062(7) -0.006(5) -0.001(6) 0.007(5) C45 0.044(6) 0.045(6) 0.063(7) -0.006(6) 0.003(6) 0.004(5) C46 0.052(6) 0.042(6) 0.057(7) -0.003(5) 0.003(6) -0.001(5) C47 0.049(5) 0.033(5) 0.046(6) -0.001(5) 0.003(5) 0.003(5) C48 0.044(5) 0.031(5) 0.043(5) -0.002(4) 0.003(5) 0.005(4) C49 0.041(5) 0.029(5) 0.038(5) 0.011(4) 0.010(4) 0.014(4) C50 0.040(6) 0.032(5) 0.043(6) 0.013(5) 0.011(5) 0.011(4) C51 0.040(6) 0.041(6) 0.049(6) 0.018(5) 0.013(5) 0.011(5) C52 0.039(6) 0.042(6) 0.054(6) 0.012(5) 0.011(5) 0.008(5) C53 0.043(6) 0.047(6) 0.051(6) 0.006(5) 0.005(5) 0.007(5) C54 0.043(6) 0.037(6) 0.044(6) 0.013(5) 0.009(5) 0.009(5) C55 0.048(5) 0.027(4) 0.029(5) 0.007(4) 0.010(4) 0.013(4) C56 0.051(6) 0.026(5) 0.034(6) 0.004(4) 0.009(5) 0.011(5) C57 0.054(7) 0.024(5) 0.042(6) 0.001(5) 0.010(5) 0.008(5) C58 0.054(7) 0.028(5) 0.041(6) 0.013(5) 0.010(5) 0.009(5) C59 0.047(6) 0.034(5) 0.041(6) 0.010(5) 0.007(5) 0.011(5) C60 0.042(6) 0.030(5) 0.030(5) 0.008(4) 0.011(4) 0.011(5) Cu3 0.0580(13) 0.0356(10) 0.0412(11) 0.0017(8) 0.0047(9) 0.0084(9) Cl3 0.056(2) 0.036(2) 0.042(2) 0.0006(16) 0.0051(18) 0.0062(18) S5 0.062(3) 0.0320(19) 0.044(2) 0.0035(17) 0.0066(19) 0.0050(18) S6 0.086(3) 0.050(3) 0.083(4) 0.016(2) 0.015(3) 0.024(2) N7 0.061(5) 0.029(5) 0.034(5) 0.002(4) 0.010(5) 0.005(4) N8 0.065(5) 0.044(5) 0.029(5) 0.002(5) 0.007(5) 0.006(4) N9 0.043(5) 0.034(4) 0.027(5) 0.008(4) 0.008(4) 0.015(4) C61 0.055(6) 0.030(5) 0.041(6) 0.002(5) 0.012(5) 0.000(4) C62 0.054(6) 0.039(5) 0.048(6) 0.005(5) 0.010(5) 0.001(5) C63 0.052(6) 0.044(5) 0.047(6) 0.003(5) 0.007(5) 0.013(5) C64 0.057(6) 0.038(5) 0.046(6) 0.003(5) 0.000(6) 0.010(5) C65 0.056(6) 0.033(5) 0.034(6) 0.001(5) 0.000(5) 0.006(5) C66 0.061(5) 0.030(5) 0.036(5) -0.002(5) 0.002(5) 0.005(4) C67 0.063(5) 0.034(4) 0.037(5) 0.004(4) 0.008(5) 0.002(4) C68 0.065(5) 0.036(4) 0.032(5) 0.003(5) 0.008(5) 0.009(4) C69 0.066(5) 0.038(4) 0.028(5) 0.006(4) 0.009(5) 0.008(4) C70 0.066(5) 0.042(4) 0.034(5) 0.006(4) 0.009(5) 0.014(4) C71 0.066(5) 0.042(5) 0.029(5) 0.004(5) 0.009(5) 0.009(4) C72 0.062(5) 0.045(5) 0.027(6) 0.008(5) 0.010(5) 0.010(4) C73 0.065(5) 0.064(6) 0.061(7) 0.007(6) 0.005(6) 0.019(5) C74 0.072(6) 0.070(7) 0.067(7) 0.010(7) -0.002(7) 0.021(5) C75 0.069(7) 0.075(7) 0.071(8) 0.013(7) 0.001(7) 0.014(5) C76 0.064(6) 0.071(7) 0.071(8) 0.010(7) -0.002(7) 0.009(6) C77 0.063(6) 0.064(6) 0.063(7) 0.010(6) -0.003(7) 0.006(5) C78 0.060(5) 0.056(5) 0.052(6) 0.007(5) 0.004(6) 0.011(4) C79 0.065(5) 0.046(5) 0.036(5) 0.008(5) 0.002(5) 0.010(4) C80 0.073(7) 0.044(6) 0.042(6) 0.008(5) -0.002(5) 0.008(5) C81 0.073(7) 0.048(7) 0.046(6) 0.010(5) -0.012(6) 0.009(6) C82 0.071(7) 0.063(7) 0.052(7) 0.005(6) -0.006(6) -0.001(6) C83 0.076(7) 0.080(8) 0.054(6) 0.012(6) 0.000(6) -0.012(6) C84 0.068(7) 0.069(7) 0.047(6) 0.012(6) -0.002(6) -0.006(6) C85 0.074(6) 0.040(4) 0.040(5) 0.010(4) 0.005(5) 0.015(5) C86 0.080(7) 0.042(5) 0.047(6) 0.007(5) -0.003(6) 0.015(6) C87 0.088(8) 0.043(6) 0.051(6) 0.007(5) 0.001(6) 0.019(6) C88 0.090(8) 0.043(6) 0.052(7) 0.013(5) 0.005(6) 0.021(6) C89 0.085(8) 0.039(6) 0.045(6) 0.017(5) 0.010(6) 0.019(6) C90 0.084(7) 0.041(5) 0.041(6) 0.012(5) 0.006(5) 0.019(6) C91 0.044(13) 0.085(12) 0.035(8) 0.001(7) 0.025(8) 0.029(6) Cl4 0.071(4) 0.049(3) 0.058(4) 0.010(2) -0.007(3) 0.023(3) Cl5 0.081(5) 0.094(5) 0.091(4) 0.051(4) 0.012(3) 0.043(4) Cl6 0.135(7) 0.053(3) 0.075(4) -0.002(3) 0.039(4) 0.005(4) O2W 0.080(5) 0.093(6) 0.089(5) 0.051(4) 0.013(4) 0.043(4) C92 0.103(6) 0.066(3) 0.066(5) -0.011(4) -0.025(4) 0.044(4) Cl7 0.105(6) 0.070(4) 0.108(6) 0.021(4) -0.035(5) 0.022(4) Cl8 0.103(6) 0.068(3) 0.066(4) -0.012(3) -0.026(4) 0.044(4) Cl9 0.062(4) 0.055(4) 0.051(4) 0.006(3) -0.002(3) 0.013(3) O1W 0.080(5) 0.093(6) 0.089(5) 0.051(4) 0.013(4) 0.043(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.899(11) . ? Cu1 N3 2.169(11) . ? Cu1 Cl1 2.192(4) . ? Cu1 N1 2.213(12) . ? Cu1 Cl2 2.693(4) . ? S1 C7 1.722(15) . ? S1 C1 1.765(14) . ? S2 C13 1.722(14) . ? S2 C12 1.738(13) . ? N1 C7 1.312(17) . ? N1 C6 1.393(17) . ? N2 C8 1.361(18) . ? N2 C11 1.363(16) . ? N3 C12 1.316(16) . ? N3 C18 1.378(18) . ? C1 C6 1.38(2) . ? C1 C2 1.381(19) . ? C2 C3 1.38(2) . ? C3 C4 1.41(2) . ? C4 C5 1.37(2) . ? C5 C6 1.385(19) . ? C7 C8 1.444(18) . ? C8 C9 1.405(18) . ? C9 C10 1.428(19) . ? C9 C19 1.52(2) . ? C10 C11 1.402(19) . ? C10 C25 1.462(18) . ? C11 C12 1.424(19) . ? C13 C14 1.38(2) . ? C13 C18 1.422(19) . ? C14 C15 1.40(2) . ? C15 C16 1.389(19) . ? C16 C17 1.37(2) . ? C17 C18 1.397(19) . ? C19 C24 1.38(2) . ? C19 C20 1.381(19) . ? C20 C21 1.38(2) . ? C21 C22 1.37(2) . ? C22 C23 1.34(2) . ? C23 C24 1.40(2) . ? C25 C26 1.38(2) . ? C25 C30 1.413(19) . ? C26 C27 1.381(18) . ? C27 C28 1.35(2) . ? C28 C29 1.39(2) . ? C29 C30 1.404(19) . ? Cu2 N5 1.875(11) . ? Cu2 Cl2 2.197(4) . ? Cu2 N6 2.200(11) . ? Cu2 N4 2.218(11) . ? Cu2 Cl3 2.654(4) . ? S3 C31 1.735(14) . ? S3 C37 1.749(14) . ? S4 C42 1.728(14) . ? S4 C43 1.749(16) . ? N4 C37 1.317(16) . ? N4 C36 1.397(16) . ? N5 C38 1.338(17) . ? N5 C41 1.359(16) . ? N6 C42 1.351(17) . ? N6 C48 1.392(18) . ? C31 C36 1.39(2) . ? C31 C32 1.41(2) . ? C32 C33 1.41(2) . ? C33 C34 1.39(2) . ? C34 C35 1.39(2) . ? C35 C36 1.403(19) . ? C37 C38 1.429(17) . ? C38 C39 1.424(17) . ? C39 C40 1.418(18) . ? C39 C49 1.487(19) . ? C40 C41 1.415(18) . ? C40 C55 1.482(17) . ? C41 C42 1.424(19) . ? C43 C44 1.37(2) . ? C43 C48 1.40(2) . ? C44 C45 1.37(2) . ? C45 C46 1.40(2) . ? C46 C47 1.37(2) . ? C47 C48 1.39(2) . ? C49 C54 1.360(19) . ? C49 C50 1.369(18) . ? C50 C51 1.412(19) . ? C51 C52 1.36(2) . ? C52 C53 1.39(2) . ? C53 C54 1.39(2) . ? C55 C56 1.394(18) . ? C55 C60 1.403(19) . ? C56 C57 1.377(18) . ? C57 C58 1.37(2) . ? C58 C59 1.366(19) . ? C59 C60 1.369(18) . ? Cu3 N8 1.880(13) . ? Cu3 N9 2.149(11) . ? Cu3 Cl3 2.203(4) . ? Cu3 S5 2.358(5) . ? S5 C67 1.697(15) . ? S6 C73 1.73(2) . ? S6 C72 1.741(16) . ? N7 C67 1.362(19) . ? N7 C66 1.436(19) . ? N8 C68 1.331(19) . ? N8 C71 1.358(19) . ? N9 C78 1.31(2) . ? N9 C72 1.371(18) . ? C61 C66 1.36(2) . ? C61 C62 1.40(2) . ? C62 C63 1.35(2) . ? C63 C64 1.42(2) . ? C64 C65 1.37(2) . ? C65 C66 1.387(19) . ? C67 C68 1.45(2) . ? C68 C69 1.42(2) . ? C69 C70 1.40(2) . ? C69 C79 1.52(2) . ? C70 C71 1.42(2) . ? C70 C85 1.51(2) . ? C71 C72 1.44(2) . ? C73 C74 1.35(2) . ? C73 C78 1.48(2) . ? C74 C75 1.44(3) . ? C75 C76 1.43(2) . ? C76 C77 1.36(2) . ? C77 C78 1.43(2) . ? C79 C84 1.34(2) . ? C79 C80 1.41(2) . ? C80 C81 1.39(2) . ? C81 C82 1.34(2) . ? C82 C83 1.33(2) . ? C83 C84 1.39(2) . ? C85 C86 1.38(2) . ? C85 C90 1.38(2) . ? C86 C87 1.37(2) . ? C87 C88 1.40(2) . ? C88 C89 1.36(2) . ? C89 C90 1.38(2) . ? C91 Cl6 1.73(3) . ? C91 Cl5 1.74(2) . ? C91 Cl4 1.77(2) . ? C92 Cl8 1.66(3) . ? C92 Cl7 1.72(3) . ? C92 Cl9 1.72(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N3 76.5(4) . . ? N2 Cu1 Cl1 170.0(4) . . ? N3 Cu1 Cl1 103.4(3) . . ? N2 Cu1 N1 75.8(4) . . ? N3 Cu1 N1 150.0(4) . . ? Cl1 Cu1 N1 102.0(3) . . ? N2 Cu1 Cl2 97.7(3) . . ? N3 Cu1 Cl2 97.6(3) . . ? Cl1 Cu1 Cl2 92.27(13) . . ? N1 Cu1 Cl2 97.2(3) . . ? C7 S1 C1 88.4(7) . . ? C13 S2 C12 90.0(7) . . ? C7 N1 C6 109.3(12) . . ? C7 N1 Cu1 111.4(9) . . ? C6 N1 Cu1 139.3(10) . . ? C8 N2 C11 109.8(11) . . ? C8 N2 Cu1 124.3(9) . . ? C11 N2 Cu1 123.7(9) . . ? C12 N3 C18 111.7(11) . . ? C12 N3 Cu1 110.8(9) . . ? C18 N3 Cu1 137.5(9) . . ? C6 C1 C2 124.0(14) . . ? C6 C1 S1 109.0(10) . . ? C2 C1 S1 127.0(12) . . ? C1 C2 C3 115.9(15) . . ? C2 C3 C4 121.3(14) . . ? C5 C4 C3 120.7(14) . . ? C4 C5 C6 119.0(15) . . ? C1 C6 C5 119.1(13) . . ? C1 C6 N1 116.1(13) . . ? C5 C6 N1 124.8(14) . . ? N1 C7 C8 117.6(13) . . ? N1 C7 S1 117.1(10) . . ? C8 C7 S1 125.2(11) . . ? N2 C8 C9 108.3(12) . . ? N2 C8 C7 110.8(12) . . ? C9 C8 C7 140.4(14) . . ? C8 C9 C10 106.7(12) . . ? C8 C9 C19 121.9(12) . . ? C10 C9 C19 130.9(12) . . ? C11 C10 C9 106.4(11) . . ? C11 C10 C25 128.9(13) . . ? C9 C10 C25 124.6(12) . . ? N2 C11 C10 108.6(12) . . ? N2 C11 C12 109.7(11) . . ? C10 C11 C12 141.1(13) . . ? N3 C12 C11 119.0(12) . . ? N3 C12 S2 114.8(10) . . ? C11 C12 S2 126.1(10) . . ? C14 C13 C18 121.7(13) . . ? C14 C13 S2 128.9(11) . . ? C18 C13 S2 109.4(11) . . ? C13 C14 C15 117.8(14) . . ? C16 C15 C14 120.3(14) . . ? C17 C16 C15 122.5(14) . . ? C16 C17 C18 118.3(13) . . ? N3 C18 C17 126.6(13) . . ? N3 C18 C13 114.1(12) . . ? C17 C18 C13 119.3(13) . . ? C24 C19 C20 119.3(14) . . ? C24 C19 C9 121.2(13) . . ? C20 C19 C9 119.5(13) . . ? C19 C20 C21 120.9(14) . . ? C22 C21 C20 119.1(15) . . ? C23 C22 C21 120.4(15) . . ? C22 C23 C24 121.7(15) . . ? C19 C24 C23 118.4(14) . . ? C26 C25 C30 115.7(13) . . ? C26 C25 C10 122.0(13) . . ? C30 C25 C10 122.1(13) . . ? C27 C26 C25 123.8(14) . . ? C28 C27 C26 119.8(16) . . ? C27 C28 C29 119.9(14) . . ? C28 C29 C30 120.2(14) . . ? C29 C30 C25 120.5(15) . . ? N5 Cu2 Cl2 169.1(3) . . ? N5 Cu2 N6 77.4(5) . . ? Cl2 Cu2 N6 102.5(3) . . ? N5 Cu2 N4 75.7(4) . . ? Cl2 Cu2 N4 104.0(3) . . ? N6 Cu2 N4 153.1(4) . . ? N5 Cu2 Cl3 94.6(3) . . ? Cl2 Cu2 Cl3 96.22(14) . . ? N6 Cu2 Cl3 90.3(3) . . ? N4 Cu2 Cl3 91.7(3) . . ? Cu2 Cl2 Cu1 93.94(13) . . ? C31 S3 C37 89.4(7) . . ? C42 S4 C43 89.6(7) . . ? C37 N4 C36 113.2(12) . . ? C37 N4 Cu2 109.4(8) . . ? C36 N4 Cu2 137.5(9) . . ? C38 N5 C41 109.9(11) . . ? C38 N5 Cu2 125.3(9) . . ? C41 N5 Cu2 123.0(9) . . ? C42 N6 C48 110.1(11) . . ? C42 N6 Cu2 109.4(9) . . ? C48 N6 Cu2 140.4(9) . . ? C36 C31 C32 122.0(14) . . ? C36 C31 S3 111.2(10) . . ? C32 C31 S3 126.8(13) . . ? C31 C32 C33 115.0(15) . . ? C34 C33 C32 122.9(14) . . ? C33 C34 C35 121.6(14) . . ? C34 C35 C36 116.1(15) . . ? C31 C36 N4 112.7(12) . . ? C31 C36 C35 122.4(13) . . ? N4 C36 C35 124.9(14) . . ? N4 C37 C38 118.7(12) . . ? N4 C37 S3 113.5(10) . . ? C38 C37 S3 127.8(10) . . ? N5 C38 C39 109.7(11) . . ? N5 C38 C37 110.0(11) . . ? C39 C38 C37 140.2(13) . . ? C40 C39 C38 105.0(11) . . ? C40 C39 C49 127.3(11) . . ? C38 C39 C49 127.7(12) . . ? C41 C40 C39 107.4(11) . . ? C41 C40 C55 125.9(12) . . ? C39 C40 C55 126.3(12) . . ? N5 C41 C40 108.0(12) . . ? N5 C41 C42 112.2(11) . . ? C40 C41 C42 139.7(12) . . ? N6 C42 C41 117.3(12) . . ? N6 C42 S4 115.3(11) . . ? C41 C42 S4 127.4(10) . . ? C44 C43 C48 122.4(15) . . ? C44 C43 S4 127.8(12) . . ? C48 C43 S4 109.8(11) . . ? C45 C44 C43 117.8(15) . . ? C44 C45 C46 120.1(16) . . ? C47 C46 C45 122.4(16) . . ? C46 C47 C48 117.7(15) . . ? C47 C48 N6 125.3(13) . . ? C47 C48 C43 119.6(14) . . ? N6 C48 C43 115.1(13) . . ? C54 C49 C50 119.8(14) . . ? C54 C49 C39 121.5(12) . . ? C50 C49 C39 118.5(13) . . ? C49 C50 C51 120.0(14) . . ? C52 C51 C50 119.3(14) . . ? C51 C52 C53 120.8(15) . . ? C54 C53 C52 118.6(15) . . ? C49 C54 C53 121.3(14) . . ? C56 C55 C60 118.1(12) . . ? C56 C55 C40 121.5(12) . . ? C60 C55 C40 120.4(12) . . ? C57 C56 C55 120.0(14) . . ? C58 C57 C56 121.1(13) . . ? C59 C58 C57 119.4(13) . . ? C58 C59 C60 121.0(14) . . ? C59 C60 C55 120.3(13) . . ? N8 Cu3 N9 80.2(5) . . ? N8 Cu3 Cl3 176.7(4) . . ? N9 Cu3 Cl3 102.8(3) . . ? N8 Cu3 S5 82.1(4) . . ? N9 Cu3 S5 162.2(3) . . ? Cl3 Cu3 S5 95.02(15) . . ? Cu3 Cl3 Cu2 110.88(16) . . ? C67 S5 Cu3 97.9(6) . . ? C73 S6 C72 90.9(8) . . ? C67 N7 C66 132.5(12) . . ? C68 N8 C71 110.6(13) . . ? C68 N8 Cu3 127.7(11) . . ? C71 N8 Cu3 121.3(11) . . ? C78 N9 C72 111.7(13) . . ? C78 N9 Cu3 139.7(11) . . ? C72 N9 Cu3 107.7(9) . . ? C66 C61 C62 119.5(14) . . ? C63 C62 C61 120.2(15) . . ? C62 C63 C64 120.7(15) . . ? C65 C64 C63 118.6(14) . . ? C64 C65 C66 120.3(15) . . ? C61 C66 C65 120.6(15) . . ? C61 C66 N7 113.7(13) . . ? C65 C66 N7 125.6(14) . . ? N7 C67 C68 116.7(13) . . ? N7 C67 S5 125.6(12) . . ? C68 C67 S5 117.6(12) . . ? N8 C68 C69 108.8(14) . . ? N8 C68 C67 114.5(13) . . ? C69 C68 C67 136.5(15) . . ? C70 C69 C68 106.2(14) . . ? C70 C69 C79 127.3(13) . . ? C68 C69 C79 125.9(14) . . ? C69 C70 C71 106.8(13) . . ? C69 C70 C85 125.4(15) . . ? C71 C70 C85 127.6(15) . . ? N8 C71 C70 107.5(14) . . ? N8 C71 C72 111.6(14) . . ? C70 C71 C72 140.6(15) . . ? N9 C72 C71 119.0(13) . . ? N9 C72 S6 113.8(12) . . ? C71 C72 S6 127.2(12) . . ? C74 C73 C78 122.2(18) . . ? C74 C73 S6 130.5(15) . . ? C78 C73 S6 107.3(13) . . ? C73 C74 C75 118.8(18) . . ? C76 C75 C74 119.6(18) . . ? C77 C76 C75 121.8(19) . . ? C76 C77 C78 120.5(18) . . ? N9 C78 C77 126.9(16) . . ? N9 C78 C73 115.9(15) . . ? C77 C78 C73 117.1(16) . . ? C84 C79 C80 119.1(16) . . ? C84 C79 C69 120.4(14) . . ? C80 C79 C69 120.6(14) . . ? C81 C80 C79 119.4(16) . . ? C82 C81 C80 120.3(16) . . ? C83 C82 C81 119.2(18) . . ? C82 C83 C84 123.3(18) . . ? C79 C84 C83 118.7(17) . . ? C86 C85 C90 118.2(14) . . ? C86 C85 C70 121.1(14) . . ? C90 C85 C70 120.7(14) . . ? C87 C86 C85 121.2(16) . . ? C86 C87 C88 120.0(16) . . ? C89 C88 C87 119.2(15) . . ? C88 C89 C90 120.3(16) . . ? C85 C90 C89 121.0(16) . . ? Cl6 C91 Cl5 108.3(14) . . ? Cl6 C91 Cl4 109.5(13) . . ? Cl5 C91 Cl4 111.1(11) . . ? Cl8 C92 Cl7 120.0(17) . . ? Cl8 C92 Cl9 115.0(14) . . ? Cl7 C92 Cl9 113.9(15) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.470 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.156 _iucr_refine_instruction_details ; TITL 2010acc1121 in P-1 CELL 0.71073 13.4166 15.8954 19.7847 96.701 95.457 95.884 ZERR 2.00 0.0009 0.0010 0.0013 0.004 0.004 0.004 LATT 1 SFAC C H N S CL CU O UNIT 182.8 114.8 18 12 14.4 6 1.2 MERG 2 SHEL 7 0.84 SIMU 0.01 $C $N $S DELU 0.01 $C $N $S SIMU 0.001 C91 C92 CL4 CL5 CL6 CL7 CL8 O1W O2W DELU 0.001 C91 C92 CL4 CL5 CL6 CL7 CL8 O1W O2W EADP O1W O2W FMAP 2 SIZE 0.12 0.08 0.02 PLAN 20 ACTA 55.00 BOND L.S. 4 WGHT 0.000000 121.455002 FVAR 0.14499 MOLE 1 CU1 6 0.325450 0.466152 0.363532 11.00000 0.03967 0.02514 = 0.03859 0.01022 0.00144 0.00647 CL1 5 0.382315 0.590910 0.336853 11.00000 0.04856 0.02376 = 0.04518 0.00780 0.00062 0.00396 S1 4 -0.016336 0.404631 0.374058 11.00000 0.03845 0.03668 = 0.04373 0.01079 0.00639 0.00861 S2 4 0.532842 0.314407 0.486367 11.00000 0.03782 0.02872 = 0.04028 0.01179 0.00088 0.00662 N1 3 0.160439 0.470285 0.350475 11.00000 0.04373 0.02962 = 0.03848 -0.00015 0.00716 0.01304 N2 3 0.272023 0.368910 0.401269 11.00000 0.04340 0.02491 = 0.03581 0.00948 0.00142 0.00891 N3 3 0.457295 0.424055 0.415884 11.00000 0.04573 0.01964 = 0.03155 0.00247 0.01055 0.01270 C1 1 -0.008584 0.496433 0.331612 11.00000 0.04745 0.03429 = 0.03979 0.00951 0.00034 0.00888 C2 1 -0.087324 0.539846 0.310038 11.00000 0.04560 0.04195 = 0.05188 0.01078 0.00139 0.01351 AFIX 43 H2 2 -0.153782 0.522088 0.316013 11.00000 -1.20000 AFIX 0 C3 1 -0.061345 0.611281 0.279030 11.00000 0.04995 0.04355 = 0.06022 0.01948 -0.00120 0.02266 AFIX 43 H3 2 -0.111596 0.642740 0.263474 11.00000 -1.20000 AFIX 0 C4 1 0.039501 0.637348 0.270531 11.00000 0.05370 0.04295 = 0.05995 0.02266 -0.00079 0.01035 AFIX 43 H4 2 0.054973 0.685506 0.249283 11.00000 -1.20000 AFIX 0 C5 1 0.115186 0.592623 0.293189 11.00000 0.04711 0.03592 = 0.05738 0.01516 -0.00145 0.00665 AFIX 43 H5 2 0.181960 0.610542 0.288157 11.00000 -1.20000 AFIX 0 C6 1 0.090760 0.520258 0.323727 11.00000 0.04555 0.03382 = 0.04435 0.00970 0.00084 0.00963 C7 1 0.112642 0.407575 0.376496 11.00000 0.04120 0.03262 = 0.03517 0.00311 0.00503 0.00996 C8 1 0.172572 0.349327 0.408006 11.00000 0.04287 0.02863 = 0.03485 0.00542 0.00443 0.00790 C9 1 0.163755 0.284640 0.450518 11.00000 0.04257 0.02699 = 0.03406 0.00568 0.00120 0.00205 C10 1 0.263800 0.268627 0.472305 11.00000 0.04190 0.02604 = 0.03667 0.00694 0.00837 0.00943 C11 1 0.328689 0.323479 0.441315 11.00000 0.04123 0.02460 = 0.03201 0.00469 0.00803 0.00990 C12 1 0.432445 0.355005 0.444118 11.00000 0.04226 0.02348 = 0.02785 0.00507 0.00998 0.01238 C13 1 0.614399 0.396423 0.466272 11.00000 0.04736 0.02697 = 0.03399 -0.00177 0.00722 0.00720 C14 1 0.717304 0.413569 0.483379 11.00000 0.04577 0.03197 = 0.03983 -0.00383 0.00835 0.00981 AFIX 43 H14 2 0.752589 0.378541 0.508978 11.00000 -1.20000 AFIX 0 C15 1 0.766674 0.485233 0.460984 11.00000 0.04358 0.03518 = 0.04061 -0.00487 0.00664 0.00983 AFIX 43 H15 2 0.835936 0.498472 0.471729 11.00000 -1.20000 AFIX 0 C16 1 0.712786 0.536809 0.422740 11.00000 0.04796 0.03520 = 0.03894 0.00120 0.00927 0.00826 AFIX 43 H16 2 0.747162 0.584610 0.408954 11.00000 -1.20000 AFIX 0 C17 1 0.610822 0.519952 0.404525 11.00000 0.04591 0.02886 = 0.04100 0.00543 0.00753 0.01203 AFIX 43 H17 2 0.576737 0.554769 0.377997 11.00000 -1.20000 AFIX 0 C18 1 0.559524 0.449146 0.426852 11.00000 0.04467 0.02369 = 0.03855 0.00122 0.01080 0.01097 C19 1 0.062919 0.251542 0.472248 11.00000 0.04295 0.02987 = 0.03624 0.00988 0.00170 0.00405 C20 1 0.013786 0.174347 0.440735 11.00000 0.04368 0.03374 = 0.03583 0.00802 -0.00037 0.00443 AFIX 43 H20 2 0.043883 0.142450 0.407589 11.00000 -1.20000 AFIX 0 C21 1 -0.079529 0.143836 0.457786 11.00000 0.04609 0.04157 = 0.04719 0.00789 0.00001 0.00238 AFIX 43 H21 2 -0.113210 0.092712 0.435275 11.00000 -1.20000 AFIX 0 C22 1 -0.121657 0.189782 0.508162 11.00000 0.04139 0.04538 = 0.04678 0.01537 0.00389 0.00591 AFIX 43 H22 2 -0.183290 0.168791 0.521145 11.00000 -1.20000 AFIX 0 C23 1 -0.074887 0.264638 0.538872 11.00000 0.04579 0.03986 = 0.04555 0.01337 0.00814 0.00946 AFIX 43 H23 2 -0.105652 0.295663 0.572158 11.00000 -1.20000 AFIX 0 C24 1 0.019084 0.297580 0.522301 11.00000 0.05035 0.03635 = 0.04107 0.00975 0.00445 0.00539 AFIX 43 H24 2 0.051198 0.349398 0.544593 11.00000 -1.20000 AFIX 0 C25 1 0.288885 0.208430 0.520036 11.00000 0.04360 0.03010 = 0.04246 0.01284 0.01379 0.01123 C26 1 0.360785 0.230832 0.575975 11.00000 0.04375 0.03781 = 0.04441 0.02288 0.01281 0.01127 AFIX 43 H26 2 0.390981 0.286915 0.584224 11.00000 -1.20000 AFIX 0 C27 1 0.390268 0.174732 0.620237 11.00000 0.04785 0.04656 = 0.05167 0.02455 0.01068 0.01279 AFIX 43 H27 2 0.440590 0.192856 0.656155 11.00000 -1.20000 AFIX 0 C28 1 0.345952 0.093732 0.611238 11.00000 0.04833 0.04117 = 0.05070 0.02335 0.02039 0.01854 AFIX 43 H28 2 0.363049 0.056596 0.642321 11.00000 -1.20000 AFIX 0 C29 1 0.274477 0.065665 0.555310 11.00000 0.05391 0.03464 = 0.05403 0.02005 0.01927 0.00738 AFIX 43 H29 2 0.245219 0.009288 0.548360 11.00000 -1.20000 AFIX 0 C30 1 0.246449 0.122231 0.509377 11.00000 0.04865 0.03063 = 0.04508 0.01102 0.01425 0.01090 AFIX 43 H30 2 0.199593 0.102812 0.471646 11.00000 -1.20000 AFIX 0 MOLE 2 CU2 6 0.287125 0.261026 0.261488 11.00000 0.04735 0.02408 = 0.03514 0.00764 0.00399 0.00867 CL2 5 0.341844 0.387997 0.237418 11.00000 0.05440 0.02170 = 0.04152 0.00486 0.00422 0.00392 S3 4 -0.052803 0.171736 0.246322 11.00000 0.04020 0.03931 = 0.03780 0.00790 0.00009 0.01237 S4 4 0.504736 0.093713 0.360813 11.00000 0.03857 0.03202 = 0.05559 0.00816 0.00301 0.01215 N4 3 0.121045 0.253380 0.239299 11.00000 0.04748 0.02597 = 0.02587 0.00682 0.00286 0.01224 N5 3 0.238201 0.163516 0.298449 11.00000 0.04574 0.02435 = 0.02931 0.00580 0.00597 0.01145 N6 3 0.426244 0.215060 0.303669 11.00000 0.04216 0.02786 = 0.03897 0.00740 0.00342 0.00892 C31 1 -0.047449 0.265195 0.208762 11.00000 0.05703 0.03081 = 0.03581 0.00388 -0.00157 0.01623 C32 1 -0.129505 0.302332 0.179906 11.00000 0.06234 0.03815 = 0.04177 0.00513 -0.00352 0.01783 AFIX 43 H32 2 -0.195918 0.278423 0.179057 11.00000 -1.20000 AFIX 0 C33 1 -0.103575 0.378431 0.152393 11.00000 0.06185 0.03482 = 0.05034 0.00595 -0.00764 0.02128 AFIX 43 H33 2 -0.154918 0.405155 0.131998 11.00000 -1.20000 AFIX 0 C34 1 -0.004806 0.415321 0.154364 11.00000 0.06642 0.02958 = 0.05192 0.00513 -0.00456 0.01594 AFIX 43 H34 2 0.007769 0.466418 0.136413 11.00000 -1.20000 AFIX 0 C35 1 0.075896 0.377624 0.182585 11.00000 0.05760 0.02688 = 0.04457 0.00815 -0.00296 0.01580 AFIX 43 H35 2 0.142315 0.401343 0.183084 11.00000 -1.20000 AFIX 0 C36 1 0.051189 0.301796 0.210218 11.00000 0.05496 0.02881 = 0.03391 0.00426 0.00110 0.01778 C37 1 0.078911 0.183458 0.259533 11.00000 0.04304 0.02780 = 0.02586 0.00749 0.00334 0.00804 C38 1 0.142342 0.127838 0.289708 11.00000 0.04261 0.02332 = 0.02831 0.00342 0.00776 0.01241 C39 1 0.136844 0.045017 0.310822 11.00000 0.04361 0.01903 = 0.02918 -0.00100 0.01210 0.01246 C40 1 0.237720 0.034163 0.333397 11.00000 0.04538 0.02067 = 0.02786 0.00322 0.00776 0.00900 C41 1 0.299125 0.108645 0.323623 11.00000 0.04182 0.02502 = 0.03045 0.00594 0.00650 0.00993 C42 1 0.402954 0.140804 0.328699 11.00000 0.04316 0.02891 = 0.03630 0.00455 0.00211 0.00844 C43 1 0.586056 0.178800 0.341691 11.00000 0.04253 0.03243 = 0.05126 -0.00368 -0.00186 0.00677 C44 1 0.689504 0.190353 0.352317 11.00000 0.04206 0.04190 = 0.06202 -0.00589 -0.00077 0.00681 AFIX 43 H44 2 0.725342 0.150300 0.371493 11.00000 -1.20000 AFIX 0 C45 1 0.738215 0.262871 0.333727 11.00000 0.04407 0.04465 = 0.06315 -0.00642 0.00336 0.00431 AFIX 43 H45 2 0.808109 0.273297 0.341310 11.00000 -1.20000 AFIX 0 C46 1 0.682942 0.321079 0.303415 11.00000 0.05209 0.04217 = 0.05707 -0.00275 0.00333 -0.00101 AFIX 43 H46 2 0.717364 0.369533 0.290651 11.00000 -1.20000 AFIX 0 C47 1 0.579839 0.309370 0.291806 11.00000 0.04886 0.03317 = 0.04572 -0.00075 0.00341 0.00329 AFIX 43 H47 2 0.544351 0.348776 0.271444 11.00000 -1.20000 AFIX 0 C48 1 0.530244 0.236783 0.311450 11.00000 0.04362 0.03114 = 0.04261 -0.00162 0.00309 0.00525 C49 1 0.045063 -0.015431 0.312223 11.00000 0.04090 0.02851 = 0.03834 0.01133 0.00991 0.01425 C50 1 0.033769 -0.053409 0.370120 11.00000 0.04046 0.03154 = 0.04258 0.01341 0.01058 0.01058 AFIX 43 H50 2 0.081687 -0.039615 0.408028 11.00000 -1.20000 AFIX 0 C51 1 -0.050628 -0.113510 0.372259 11.00000 0.03974 0.04063 = 0.04945 0.01819 0.01270 0.01131 AFIX 43 H51 2 -0.060050 -0.137847 0.412036 11.00000 -1.20000 AFIX 0 C52 1 -0.117955 -0.135415 0.315559 11.00000 0.03942 0.04154 = 0.05371 0.01187 0.01055 0.00825 AFIX 43 H52 2 -0.173263 -0.175442 0.316580 11.00000 -1.20000 AFIX 0 C53 1 -0.105216 -0.098780 0.256095 11.00000 0.04295 0.04683 = 0.05079 0.00614 0.00537 0.00691 AFIX 43 H53 2 -0.150330 -0.115073 0.216959 11.00000 -1.20000 AFIX 0 C54 1 -0.023775 -0.037363 0.256294 11.00000 0.04298 0.03716 = 0.04380 0.01253 0.00869 0.00899 AFIX 43 H54 2 -0.016142 -0.010683 0.217395 11.00000 -1.20000 AFIX 0 C55 1 0.273944 -0.044706 0.354808 11.00000 0.04789 0.02659 = 0.02922 0.00666 0.01047 0.01326 C56 1 0.240489 -0.124542 0.318157 11.00000 0.05079 0.02623 = 0.03378 0.00449 0.00928 0.01099 AFIX 43 H56 2 0.191317 -0.129558 0.281016 11.00000 -1.20000 AFIX 0 C57 1 0.280233 -0.195951 0.336938 11.00000 0.05362 0.02383 = 0.04166 0.00108 0.00977 0.00769 AFIX 43 H57 2 0.259596 -0.248602 0.311051 11.00000 -1.20000 AFIX 0 C58 1 0.349670 -0.190716 0.393127 11.00000 0.05427 0.02822 = 0.04079 0.01321 0.00997 0.00893 AFIX 43 H58 2 0.373899 -0.239717 0.406413 11.00000 -1.20000 AFIX 0 C59 1 0.383004 -0.112874 0.429468 11.00000 0.04727 0.03382 = 0.04107 0.00973 0.00703 0.01089 AFIX 43 H59 2 0.431092 -0.109109 0.467115 11.00000 -1.20000 AFIX 0 C60 1 0.346732 -0.040306 0.411341 11.00000 0.04216 0.02972 = 0.03034 0.00778 0.01096 0.01092 AFIX 43 H60 2 0.370445 0.012164 0.436616 11.00000 -1.20000 AFIX 0 MOLE 3 CU3 6 0.234499 0.044608 0.131187 11.00000 0.05795 0.03563 = 0.04123 0.00169 0.00471 0.00837 CL3 5 0.303606 0.177770 0.139490 11.00000 0.05604 0.03649 = 0.04240 0.00058 0.00507 0.00624 S5 4 0.069214 0.075484 0.100662 11.00000 0.06155 0.03197 = 0.04370 0.00347 0.00665 0.00498 S6 4 0.422490 -0.172627 0.163237 11.00000 0.08592 0.05040 = 0.08253 0.01554 0.01537 0.02351 N7 3 -0.088952 -0.049475 0.070342 11.00000 0.06076 0.02938 = 0.03385 0.00193 0.00984 0.00464 AFIX 43 H7 2 -0.106495 -0.103249 0.069161 11.00000 -1.20000 AFIX 0 N8 3 0.169682 -0.067493 0.120553 11.00000 0.06534 0.04359 = 0.02931 0.00240 0.00657 0.00646 N9 3 0.361011 -0.022560 0.157026 11.00000 0.04335 0.03401 = 0.02729 0.00830 0.00756 0.01494 C61 1 -0.258624 -0.051529 0.028218 11.00000 0.05478 0.02962 = 0.04118 0.00195 0.01210 -0.00033 AFIX 43 H61 2 -0.260715 -0.110615 0.022457 11.00000 -1.20000 AFIX 0 C62 1 -0.344573 -0.013188 0.010102 11.00000 0.05377 0.03860 = 0.04838 0.00513 0.01037 0.00119 AFIX 43 H62 2 -0.404718 -0.046840 -0.006451 11.00000 -1.20000 AFIX 0 C63 1 -0.340738 0.072294 0.016498 11.00000 0.05184 0.04402 = 0.04720 0.00275 0.00743 0.01282 AFIX 43 H63 2 -0.398175 0.097324 0.003765 11.00000 -1.20000 AFIX 0 C64 1 -0.250070 0.124634 0.042442 11.00000 0.05741 0.03817 = 0.04606 0.00314 -0.00028 0.00975 AFIX 43 H64 2 -0.247304 0.183735 0.046631 11.00000 -1.20000 AFIX 0 C65 1 -0.166873 0.086419 0.061152 11.00000 0.05580 0.03268 = 0.03448 0.00067 0.00027 0.00579 AFIX 43 H65 2 -0.106785 0.119688 0.078489 11.00000 -1.20000 AFIX 0 C66 1 -0.171562 -0.001802 0.054419 11.00000 0.06128 0.03019 = 0.03569 -0.00209 0.00249 0.00527 C67 1 0.011756 -0.026123 0.086946 11.00000 0.06288 0.03365 = 0.03670 0.00445 0.00834 0.00151 C68 1 0.073417 -0.094006 0.098718 11.00000 0.06495 0.03638 = 0.03249 0.00269 0.00752 0.00919 C69 1 0.060375 -0.184643 0.088098 11.00000 0.06625 0.03821 = 0.02839 0.00639 0.00892 0.00839 C70 1 0.154722 -0.210481 0.107658 11.00000 0.06622 0.04194 = 0.03378 0.00632 0.00884 0.01412 C71 1 0.222465 -0.134917 0.127995 11.00000 0.06598 0.04186 = 0.02912 0.00372 0.00943 0.00897 C72 1 0.327609 -0.107958 0.148405 11.00000 0.06153 0.04504 = 0.02748 0.00815 0.01034 0.01028 C73 1 0.512318 -0.084658 0.178576 11.00000 0.06526 0.06369 = 0.06129 0.00742 0.00500 0.01925 C74 1 0.612875 -0.079099 0.194767 11.00000 0.07231 0.07034 = 0.06689 0.01004 -0.00179 0.02081 AFIX 43 H74 2 0.644243 -0.127764 0.200244 11.00000 -1.20000 AFIX 0 C75 1 0.670820 0.003575 0.203425 11.00000 0.06950 0.07472 = 0.07150 0.01336 0.00080 0.01385 AFIX 43 H75 2 0.740023 0.009069 0.215822 11.00000 -1.20000 AFIX 0 C76 1 0.621370 0.077018 0.192858 11.00000 0.06386 0.07105 = 0.07100 0.01033 -0.00241 0.00914 AFIX 43 H76 2 0.659547 0.129978 0.197134 11.00000 -1.20000 AFIX 0 C77 1 0.520254 0.071666 0.176758 11.00000 0.06312 0.06447 = 0.06313 0.00996 -0.00289 0.00607 AFIX 43 H77 2 0.490139 0.120793 0.170674 11.00000 -1.20000 AFIX 0 C78 1 0.459671 -0.008690 0.169072 11.00000 0.06002 0.05646 = 0.05235 0.00727 0.00397 0.01094 C79 1 -0.039439 -0.240818 0.069569 11.00000 0.06518 0.04572 = 0.03596 0.00844 0.00199 0.01038 C80 1 -0.086529 -0.253439 0.001695 11.00000 0.07288 0.04415 = 0.04217 0.00830 -0.00153 0.00766 AFIX 43 H80 2 -0.056236 -0.228106 -0.032419 11.00000 -1.20000 AFIX 0 C81 1 -0.178679 -0.304113 -0.013748 11.00000 0.07320 0.04831 = 0.04580 0.01032 -0.01224 0.00933 AFIX 43 H81 2 -0.210807 -0.311655 -0.058156 11.00000 -1.20000 AFIX 0 C82 1 -0.221359 -0.342132 0.035164 11.00000 0.07115 0.06266 = 0.05174 0.00512 -0.00648 -0.00089 AFIX 43 H82 2 -0.281623 -0.377785 0.024585 11.00000 -1.20000 AFIX 0 C83 1 -0.176410 -0.328189 0.098938 11.00000 0.07577 0.07956 = 0.05427 0.01185 -0.00006 -0.01238 AFIX 43 H83 2 -0.207413 -0.353996 0.132553 11.00000 -1.20000 AFIX 0 C84 1 -0.085404 -0.276978 0.117896 11.00000 0.06795 0.06919 = 0.04655 0.01189 -0.00226 -0.00565 AFIX 43 H84 2 -0.057000 -0.268007 0.163257 11.00000 -1.20000 AFIX 0 C85 1 0.178807 -0.301470 0.102681 11.00000 0.07380 0.04016 = 0.04046 0.00980 0.00461 0.01499 C86 1 0.144526 -0.358821 0.045536 11.00000 0.08034 0.04198 = 0.04729 0.00691 -0.00336 0.01478 AFIX 43 H86 2 0.104686 -0.341458 0.009829 11.00000 -1.20000 AFIX 0 C87 1 0.168030 -0.440886 0.040354 11.00000 0.08755 0.04325 = 0.05092 0.00703 0.00080 0.01852 AFIX 43 H87 2 0.145197 -0.478477 0.001027 11.00000 -1.20000 AFIX 0 C88 1 0.226366 -0.468286 0.094153 11.00000 0.09004 0.04265 = 0.05188 0.01264 0.00519 0.02080 AFIX 43 H88 2 0.240144 -0.524654 0.091739 11.00000 -1.20000 AFIX 0 C89 1 0.262627 -0.411667 0.149913 11.00000 0.08521 0.03922 = 0.04508 0.01660 0.00969 0.01925 AFIX 43 H89 2 0.304656 -0.428431 0.184793 11.00000 -1.20000 AFIX 0 C90 1 0.237392 -0.329140 0.155133 11.00000 0.08419 0.04093 = 0.04079 0.01202 0.00618 0.01901 AFIX 43 H90 2 0.260188 -0.291681 0.194540 11.00000 -1.20000 AFIX 0 MOLE 4 PART 1 C91 1 0.578160 0.583790 0.214686 10.70000 0.04443 0.08527 = 0.03451 0.00099 0.02532 0.02931 AFIX 13 H91 2 0.518686 0.565391 0.236722 10.70000 -1.20000 AFIX 0 CL4 5 0.651518 0.498273 0.202585 10.70000 0.07134 0.04896 = 0.05793 0.00965 -0.00707 0.02292 CL5 5 0.539662 0.618141 0.137020 10.70000 0.08107 0.09399 = 0.09055 0.05071 0.01237 0.04310 CL6 5 0.648789 0.668384 0.266423 10.70000 0.13464 0.05343 = 0.07506 -0.00209 0.03912 0.00453 PART 2 O2W 7 0.492715 0.540414 0.117331 10.30000 0.08001 0.09315 = 0.08939 0.05146 0.01287 0.04276 MOLE 5 PART 3 C92 1 0.507504 0.691618 -0.063297 10.70000 0.10347 0.06562 = 0.06626 -0.01144 -0.02503 0.04448 AFIX 13 H92 2 0.563716 0.705000 -0.089925 10.70000 -1.20000 AFIX 0 CL7 5 0.518565 0.586899 -0.054065 10.70000 0.10536 0.06953 = 0.10775 0.02056 -0.03529 0.02169 CL8 5 0.411588 0.716625 -0.113129 10.70000 0.10304 0.06799 = 0.06633 -0.01235 -0.02570 0.04407 CL9 5 0.542653 0.760733 0.010604 10.70000 0.06193 0.05501 = 0.05108 0.00639 -0.00233 0.01330 PART 4 O1W 7 0.362787 0.639286 -0.015468 10.30000 0.08001 0.09315 = 0.08939 0.05146 0.01287 0.04276 HKLF 4 REM 2010acc1121 in P-1 REM R1 = 0.1559 for 8265 Fo > 4sig(Fo) and 0.2480 for all 14445 data REM 1084 parameters refined using 989 restraints END WGHT 0.0000 121.3261 REM Highest difference peak 1.470, deepest hole -0.840, 1-sigma level 0.156 Q1 1 0.5859 0.6575 0.2252 11.00000 0.05 1.47 Q2 1 0.1677 -0.0003 0.1238 11.00000 0.05 1.12 Q3 1 0.3765 0.6928 -0.0883 11.00000 0.05 0.86 Q4 1 0.4499 0.6487 -0.0540 11.00000 0.05 0.75 Q5 1 0.4603 0.7475 -0.1018 11.00000 0.05 0.74 Q6 1 0.3522 -0.2019 0.1404 11.00000 0.05 0.73 Q7 1 0.6059 0.4780 0.1627 11.00000 0.05 0.72 Q8 1 0.5475 0.7020 -0.0162 11.00000 0.05 0.69 Q9 1 0.2244 0.2213 0.2479 11.00000 0.05 0.69 Q10 1 0.5293 0.7165 -0.0261 11.00000 0.05 0.69 Q11 1 0.2800 0.2117 0.3127 11.00000 0.05 0.67 Q12 1 0.2657 0.4211 0.3598 11.00000 0.05 0.66 Q13 1 0.5243 0.1464 0.3288 11.00000 0.05 0.64 Q14 1 0.4489 0.1137 0.3560 11.00000 0.05 0.64 Q15 1 0.5736 0.7165 0.0034 11.00000 0.05 0.62 Q16 1 0.4287 -0.0224 0.2751 11.00000 0.05 0.62 Q17 1 0.2388 0.1363 0.1258 11.00000 0.05 0.62 Q18 1 0.7610 0.4594 0.5000 11.00000 0.05 0.61 Q19 1 0.6748 0.5290 0.1618 11.00000 0.05 0.61 Q20 1 0.4267 0.7019 -0.1379 11.00000 0.05 0.61 ; #===END data_2010acc1121b_complex_7 _database_code_depnum_ccdc_archive 'CCDC 817765' #TrackingRef '- Ogden_Dalton_combined.cif.txt' _chemical_compound_source 'Massimiliano Massi' _database_code_CSD 10AC1121 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H23 Cl4 Cu N3 S2' _chemical_formula_weight 706.98 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.98270(10) _cell_length_b 12.2046(2) _cell_length_c 14.5977(2) _cell_angle_alpha 79.8410(10) _cell_angle_beta 76.8820(10) _cell_angle_gamma 84.9810(10) _cell_volume 1532.27(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 43318 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Fragment _exptl_crystal_colour 'Dark Green' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 1.225 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7917 _exptl_absorpt_correction_T_max 0.9526 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28317 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7002 _reflns_number_gt 5912 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Images generated using CrystalMaker: a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd, Oxford, England (www.crystalmaker.com) ; _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.7670P] 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 7002 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Cu1 Cu 0.09577(4) 0.35944(3) 0.44380(2) 0.02106(9) Uani 1 1 d . . . Cl1 Cl 0.06875(8) 0.42977(6) 0.29842(5) 0.02314(15) Uani 1 1 d . . . S1 S -0.15807(8) 0.40388(6) 0.52048(5) 0.02372(15) Uani 1 1 d . . . S2 S 0.34970(9) 0.28543(6) 0.40072(5) 0.02635(16) Uani 1 1 d . . . N1 N -0.2580(3) 0.34381(19) 0.70887(16) 0.0211(5) Uani 1 1 d . . . H1 H -0.2405 0.3028 0.7617 0.025 Uiso 1 1 calc R . . N2 N 0.1121(3) 0.28735(18) 0.56735(16) 0.0183(5) Uani 1 1 d . . . N3 N 0.4963(3) 0.17077(19) 0.53226(17) 0.0221(5) Uani 1 1 d . . . H3 H 0.4918 0.1467 0.5933 0.027 Uiso 1 1 calc R . . C1 C -0.4963(3) 0.4054(2) 0.6526(2) 0.0261(6) Uani 1 1 d . . . H1A H -0.4611 0.3728 0.5966 0.031 Uiso 1 1 calc R . . C2 C -0.6413(3) 0.4582(2) 0.6709(2) 0.0309(7) Uani 1 1 d . . . H2 H -0.7055 0.4614 0.6269 0.037 Uiso 1 1 calc R . . C3 C -0.6931(4) 0.5059(3) 0.7522(3) 0.0333(7) Uani 1 1 d . . . H3A H -0.7926 0.5412 0.7641 0.040 Uiso 1 1 calc R . . C4 C -0.5997(3) 0.5019(3) 0.8164(2) 0.0328(7) Uani 1 1 d . . . H4 H -0.6346 0.5354 0.8720 0.039 Uiso 1 1 calc R . . C5 C -0.4556(3) 0.4494(3) 0.7996(2) 0.0276(6) Uani 1 1 d . . . H5 H -0.3919 0.4460 0.8440 0.033 Uiso 1 1 calc R . . C6 C -0.4041(3) 0.4014(2) 0.7178(2) 0.0214(6) Uani 1 1 d . . . C7 C -0.1439(3) 0.3425(2) 0.6328(2) 0.0194(5) Uani 1 1 d . . . C8 C 0.0002(3) 0.2871(2) 0.64674(19) 0.0182(5) Uani 1 1 d . . . C9 C 0.0562(3) 0.2288(2) 0.72616(19) 0.0192(5) Uani 1 1 d . . . C10 C 0.2073(3) 0.1927(2) 0.69069(19) 0.0183(5) Uani 1 1 d . . . C11 C 0.2380(3) 0.2316(2) 0.59077(19) 0.0190(5) Uani 1 1 d . . . C12 C 0.3691(3) 0.2254(2) 0.5125(2) 0.0203(5) Uani 1 1 d . . . C13 C 0.6376(3) 0.1449(2) 0.4715(2) 0.0223(6) Uani 1 1 d . . . C14 C 0.7125(3) 0.0440(2) 0.5005(2) 0.0243(6) Uani 1 1 d . . . H14 H 0.6675 -0.0037 0.5570 0.029 Uiso 1 1 calc R . . C15 C 0.8532(3) 0.0137(3) 0.4462(2) 0.0282(7) Uani 1 1 d . . . H15 H 0.9040 -0.0554 0.4651 0.034 Uiso 1 1 calc R . . C16 C 0.9199(3) 0.0840(3) 0.3645(2) 0.0304(7) Uani 1 1 d . . . H16 H 1.0164 0.0635 0.3276 0.036 Uiso 1 1 calc R . . C17 C 0.8450(3) 0.1844(3) 0.3369(2) 0.0307(7) Uani 1 1 d . . . H17 H 0.8907 0.2323 0.2808 0.037 Uiso 1 1 calc R . . C18 C 0.7040(3) 0.2159(2) 0.3901(2) 0.0259(6) Uani 1 1 d . . . H18 H 0.6537 0.2851 0.3710 0.031 Uiso 1 1 calc R . . C19 C -0.0285(3) 0.2080(2) 0.82722(19) 0.0193(5) Uani 1 1 d . . . C20 C -0.0733(3) 0.2952(2) 0.8791(2) 0.0262(6) Uani 1 1 d . . . H20 H -0.0473 0.3690 0.8501 0.031 Uiso 1 1 calc R . . C21 C -0.1555(4) 0.2753(3) 0.9724(2) 0.0319(7) Uani 1 1 d . . . H21 H -0.1858 0.3356 1.0070 0.038 Uiso 1 1 calc R . . C22 C -0.1938(3) 0.1683(3) 1.0155(2) 0.0322(7) Uani 1 1 d . . . H22 H -0.2506 0.1549 1.0795 0.039 Uiso 1 1 calc R . . C23 C -0.1491(4) 0.0817(3) 0.9655(2) 0.0350(8) Uani 1 1 d . . . H23 H -0.1748 0.0080 0.9951 0.042 Uiso 1 1 calc R . . C24 C -0.0666(4) 0.1004(2) 0.8716(2) 0.0295(7) Uani 1 1 d . . . H24 H -0.0362 0.0396 0.8378 0.035 Uiso 1 1 calc R . . C25 C 0.3144(3) 0.1305(2) 0.74826(19) 0.0197(5) Uani 1 1 d . . . C26 C 0.3551(3) 0.1787(2) 0.8183(2) 0.0236(6) Uani 1 1 d . . . H26 H 0.3118 0.2498 0.8309 0.028 Uiso 1 1 calc R . . C27 C 0.4590(4) 0.1227(3) 0.8696(2) 0.0301(7) Uani 1 1 d . . . H27 H 0.4864 0.1557 0.9173 0.036 Uiso 1 1 calc R . . C28 C 0.5232(4) 0.0190(3) 0.8520(2) 0.0311(7) Uani 1 1 d . . . H28 H 0.5955 -0.0182 0.8868 0.037 Uiso 1 1 calc R . . C29 C 0.4818(3) -0.0302(2) 0.7838(2) 0.0268(6) Uani 1 1 d . . . H29 H 0.5251 -0.1015 0.7719 0.032 Uiso 1 1 calc R . . C30 C 0.3764(3) 0.0249(2) 0.7325(2) 0.0230(6) Uani 1 1 d . . . H30 H 0.3467 -0.0097 0.6864 0.028 Uiso 1 1 calc R . . C31 C 0.2363(4) 0.3167(3) 0.1077(2) 0.0357(8) Uani 1 1 d . . . H31 H 0.2202 0.3332 0.1741 0.043 Uiso 1 1 calc R . . Cl2 Cl 0.13995(12) 0.42206(8) 0.04188(7) 0.0500(2) Uani 1 1 d . . . Cl3 Cl 0.15892(11) 0.18826(8) 0.11309(9) 0.0610(3) Uani 1 1 d . . . Cl4 Cl 0.43417(10) 0.31137(8) 0.05860(7) 0.0426(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 Cu1 0.02600(18) 0.02053(17) 0.01589(17) -0.00081(13) -0.00525(13) 0.00068(13) Cl1 0.0286(3) 0.0244(3) 0.0167(3) -0.0016(3) -0.0065(3) -0.0021(3) S1 0.0266(4) 0.0261(4) 0.0179(3) 0.0006(3) -0.0080(3) 0.0014(3) S2 0.0280(4) 0.0296(4) 0.0182(3) -0.0003(3) -0.0028(3) 0.0035(3) N1 0.0233(12) 0.0211(11) 0.0178(11) 0.0018(9) -0.0069(9) 0.0014(9) N2 0.0219(11) 0.0158(10) 0.0162(11) -0.0014(9) -0.0041(9) 0.0025(9) N3 0.0260(12) 0.0198(11) 0.0186(12) -0.0010(9) -0.0032(10) 0.0011(10) C1 0.0287(15) 0.0225(14) 0.0278(16) 0.0032(12) -0.0122(13) -0.0046(12) C2 0.0265(15) 0.0241(15) 0.0426(19) 0.0075(13) -0.0173(14) -0.0049(12) C3 0.0209(15) 0.0262(16) 0.048(2) 0.0046(14) -0.0064(14) 0.0009(12) C4 0.0236(15) 0.0349(17) 0.0365(18) -0.0064(14) -0.0004(13) 0.0027(13) C5 0.0218(14) 0.0339(16) 0.0270(16) -0.0040(13) -0.0061(12) 0.0002(12) C6 0.0191(13) 0.0171(13) 0.0266(15) 0.0016(11) -0.0049(11) -0.0039(10) C7 0.0217(13) 0.0142(12) 0.0229(14) -0.0029(10) -0.0053(11) -0.0029(10) C8 0.0206(13) 0.0148(12) 0.0189(13) -0.0021(10) -0.0043(10) -0.0006(10) C9 0.0232(13) 0.0137(12) 0.0208(14) -0.0003(10) -0.0060(11) -0.0021(10) C10 0.0209(13) 0.0124(12) 0.0216(14) -0.0020(10) -0.0050(11) -0.0009(10) C11 0.0246(14) 0.0138(12) 0.0185(13) -0.0030(10) -0.0055(11) 0.0024(10) C12 0.0260(14) 0.0139(12) 0.0218(14) -0.0042(10) -0.0064(11) 0.0001(10) C13 0.0226(14) 0.0189(13) 0.0279(15) -0.0085(11) -0.0066(11) -0.0009(11) C14 0.0241(14) 0.0229(14) 0.0280(15) -0.0045(12) -0.0090(12) -0.0034(11) C15 0.0244(15) 0.0255(15) 0.0392(18) -0.0104(13) -0.0134(13) 0.0023(12) C16 0.0185(14) 0.0337(17) 0.0400(18) -0.0135(14) -0.0021(13) -0.0024(12) C17 0.0248(15) 0.0303(16) 0.0354(18) -0.0055(13) -0.0002(13) -0.0084(13) C18 0.0264(15) 0.0164(13) 0.0340(17) -0.0038(12) -0.0039(13) -0.0027(11) C19 0.0172(12) 0.0223(13) 0.0172(13) 0.0016(10) -0.0054(10) -0.0001(10) C20 0.0307(16) 0.0244(14) 0.0216(14) -0.0010(12) -0.0032(12) -0.0029(12) C21 0.0335(17) 0.0360(17) 0.0239(16) -0.0052(13) -0.0026(13) 0.0017(14) C22 0.0246(15) 0.0468(19) 0.0201(15) 0.0042(14) -0.0019(12) -0.0017(14) C23 0.0375(18) 0.0308(17) 0.0310(17) 0.0106(14) -0.0033(14) -0.0130(14) C24 0.0370(17) 0.0212(14) 0.0289(16) 0.0028(12) -0.0072(13) -0.0076(13) C25 0.0200(13) 0.0193(13) 0.0174(13) 0.0014(10) -0.0023(10) -0.0019(10) C26 0.0281(15) 0.0205(13) 0.0216(14) -0.0018(11) -0.0046(12) -0.0029(11) C27 0.0342(17) 0.0351(17) 0.0238(15) -0.0022(13) -0.0129(13) -0.0042(14) C28 0.0278(16) 0.0360(17) 0.0282(16) 0.0051(13) -0.0124(13) 0.0017(13) C29 0.0287(15) 0.0210(14) 0.0269(15) 0.0055(12) -0.0064(12) 0.0018(12) C30 0.0279(15) 0.0191(13) 0.0213(14) 0.0021(11) -0.0075(12) -0.0031(11) C31 0.0435(19) 0.0286(16) 0.0297(17) -0.0025(13) -0.0024(15) 0.0072(14) Cl2 0.0563(6) 0.0374(5) 0.0509(6) 0.0063(4) -0.0154(5) 0.0089(4) Cl3 0.0426(5) 0.0287(4) 0.0942(9) -0.0012(5) 0.0137(5) -0.0003(4) Cl4 0.0385(5) 0.0432(5) 0.0464(5) -0.0109(4) -0.0068(4) -0.0022(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.894(2) . ? Cu1 Cl1 2.2032(7) . ? Cu1 S1 2.3634(8) . ? Cu1 S2 2.3670(8) . ? S1 C7 1.706(3) . ? S2 C12 1.708(3) . ? N1 C7 1.331(4) . ? N1 C6 1.424(3) . ? N2 C11 1.348(3) . ? N2 C8 1.350(3) . ? N3 C12 1.335(4) . ? N3 C13 1.420(4) . ? C1 C6 1.388(4) . ? C1 C2 1.392(4) . ? C2 C3 1.383(5) . ? C3 C4 1.385(5) . ? C4 C5 1.383(4) . ? C5 C6 1.390(4) . ? C7 C8 1.447(4) . ? C8 C9 1.419(4) . ? C9 C10 1.400(4) . ? C9 C19 1.487(4) . ? C10 C11 1.423(4) . ? C10 C25 1.491(4) . ? C11 C12 1.449(4) . ? C13 C18 1.387(4) . ? C13 C14 1.396(4) . ? C14 C15 1.389(4) . ? C15 C16 1.386(4) . ? C16 C17 1.386(4) . ? C17 C18 1.388(4) . ? C19 C20 1.392(4) . ? C19 C24 1.393(4) . ? C20 C21 1.386(4) . ? C21 C22 1.382(5) . ? C22 C23 1.371(5) . ? C23 C24 1.391(4) . ? C25 C30 1.395(4) . ? C25 C26 1.396(4) . ? C26 C27 1.387(4) . ? C27 C28 1.386(5) . ? C28 C29 1.381(4) . ? C29 C30 1.394(4) . ? C31 Cl3 1.752(4) . ? C31 Cl2 1.753(3) . ? C31 Cl4 1.759(4) . ? 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 N2 Cu1 Cl1 174.97(7) . . ? N2 Cu1 S1 83.68(7) . . ? Cl1 Cu1 S1 95.91(3) . . ? N2 Cu1 S2 83.20(7) . . ? Cl1 Cu1 S2 96.89(3) . . ? S1 Cu1 S2 166.51(3) . . ? C7 S1 Cu1 96.95(10) . . ? C12 S2 Cu1 97.30(10) . . ? C7 N1 C6 129.8(2) . . ? C11 N2 C8 109.2(2) . . ? C11 N2 Cu1 125.71(19) . . ? C8 N2 Cu1 125.07(18) . . ? C12 N3 C13 130.9(2) . . ? C6 C1 C2 118.7(3) . . ? C3 C2 C1 120.9(3) . . ? C2 C3 C4 119.8(3) . . ? C5 C4 C3 120.1(3) . . ? C4 C5 C6 119.9(3) . . ? C1 C6 C5 120.6(3) . . ? C1 C6 N1 123.2(3) . . ? C5 C6 N1 116.1(2) . . ? N1 C7 C8 117.9(2) . . ? N1 C7 S1 123.6(2) . . ? C8 C7 S1 118.5(2) . . ? N2 C8 C9 109.0(2) . . ? N2 C8 C7 115.7(2) . . ? C9 C8 C7 135.2(3) . . ? C10 C9 C8 106.5(2) . . ? C10 C9 C19 126.3(2) . . ? C8 C9 C19 127.2(2) . . ? C9 C10 C11 106.2(2) . . ? C9 C10 C25 126.0(2) . . ? C11 C10 C25 127.8(2) . . ? N2 C11 C10 109.1(2) . . ? N2 C11 C12 115.6(2) . . ? C10 C11 C12 135.2(2) . . ? N3 C12 C11 117.8(2) . . ? N3 C12 S2 124.1(2) . . ? C11 C12 S2 118.0(2) . . ? C18 C13 C14 120.5(3) . . ? C18 C13 N3 123.4(3) . . ? C14 C13 N3 116.0(3) . . ? C15 C14 C13 119.6(3) . . ? C16 C15 C14 120.2(3) . . ? C17 C16 C15 119.7(3) . . ? C16 C17 C18 120.9(3) . . ? C13 C18 C17 119.1(3) . . ? C20 C19 C24 118.5(3) . . ? C20 C19 C9 121.1(2) . . ? C24 C19 C9 120.4(3) . . ? C21 C20 C19 120.6(3) . . ? C22 C21 C20 120.3(3) . . ? C23 C22 C21 119.6(3) . . ? C22 C23 C24 120.7(3) . . ? C23 C24 C19 120.2(3) . . ? C30 C25 C26 119.2(3) . . ? C30 C25 C10 121.0(2) . . ? C26 C25 C10 119.7(2) . . ? C27 C26 C25 119.9(3) . . ? C28 C27 C26 120.7(3) . . ? C29 C28 C27 119.9(3) . . ? C28 C29 C30 119.9(3) . . ? C29 C30 C25 120.4(3) . . ? Cl3 C31 Cl2 109.6(2) . . ? Cl3 C31 Cl4 110.65(18) . . ? Cl2 C31 Cl4 111.42(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.520 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.083 _iucr_refine_instruction_details ; TITL 2010acc1121b in P-1 CELL 0.71073 8.9827 12.2046 14.5977 79.841 76.882 84.981 ZERR 2.00 0.0001 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H N S CL CU UNIT 62 46 6 4 8 2 MERG 2 SHEL 7 0.77 FMAP 2 PLAN 20 SIZE 0.04 0.07 0.20 ACTA 55.00 BOND L.S. 4 TEMP -153.00 WGHT 0.000000 3.767000 FVAR 0.32930 MOLE 1 CU1 6 0.095773 0.359441 0.443797 11.00000 0.02600 0.02053 = 0.01589 -0.00081 -0.00525 0.00068 CL1 5 0.068747 0.429770 0.298424 11.00000 0.02855 0.02445 = 0.01668 -0.00157 -0.00645 -0.00212 S1 4 -0.158074 0.403881 0.520481 11.00000 0.02660 0.02613 = 0.01790 0.00065 -0.00797 0.00144 S2 4 0.349700 0.285429 0.400720 11.00000 0.02799 0.02957 = 0.01822 -0.00033 -0.00284 0.00353 N1 3 -0.258027 0.343810 0.708866 11.00000 0.02330 0.02106 = 0.01781 0.00179 -0.00690 0.00141 AFIX 43 H1 2 -0.240536 0.302817 0.761674 11.00000 -1.20000 AFIX 0 N2 3 0.112090 0.287345 0.567352 11.00000 0.02194 0.01582 = 0.01618 -0.00140 -0.00414 0.00245 N3 3 0.496303 0.170768 0.532257 11.00000 0.02604 0.01977 = 0.01858 -0.00102 -0.00321 0.00109 AFIX 43 H3 2 0.491844 0.146735 0.593261 11.00000 -1.20000 AFIX 0 C1 1 -0.496283 0.405437 0.652597 11.00000 0.02874 0.02251 = 0.02775 0.00322 -0.01219 -0.00455 AFIX 43 H1A 2 -0.461067 0.372816 0.596585 11.00000 -1.20000 AFIX 0 C2 1 -0.641320 0.458163 0.670883 11.00000 0.02649 0.02412 = 0.04259 0.00752 -0.01731 -0.00491 AFIX 43 H2 2 -0.705536 0.461405 0.626863 11.00000 -1.20000 AFIX 0 C3 1 -0.693148 0.505871 0.752249 11.00000 0.02088 0.02621 = 0.04795 0.00461 -0.00640 0.00087 AFIX 43 H3A 2 -0.792559 0.541244 0.764111 11.00000 -1.20000 AFIX 0 C4 1 -0.599662 0.501919 0.816402 11.00000 0.02355 0.03488 = 0.03653 -0.00642 -0.00043 0.00274 AFIX 43 H4 2 -0.634553 0.535354 0.872003 11.00000 -1.20000 AFIX 0 C5 1 -0.455584 0.449360 0.799614 11.00000 0.02179 0.03392 = 0.02696 -0.00397 -0.00614 0.00024 AFIX 43 H5 2 -0.391896 0.446015 0.843951 11.00000 -1.20000 AFIX 0 C6 1 -0.404133 0.401446 0.717769 11.00000 0.01913 0.01711 = 0.02655 0.00165 -0.00492 -0.00392 C7 1 -0.143933 0.342545 0.632791 11.00000 0.02170 0.01421 = 0.02291 -0.00288 -0.00530 -0.00294 C8 1 0.000224 0.287081 0.646739 11.00000 0.02061 0.01475 = 0.01888 -0.00211 -0.00431 -0.00056 C9 1 0.056214 0.228778 0.726159 11.00000 0.02319 0.01365 = 0.02079 -0.00033 -0.00599 -0.00212 C10 1 0.207265 0.192713 0.690690 11.00000 0.02090 0.01244 = 0.02157 -0.00205 -0.00496 -0.00093 C11 1 0.238003 0.231586 0.590774 11.00000 0.02456 0.01377 = 0.01845 -0.00296 -0.00545 0.00243 C12 1 0.369063 0.225409 0.512548 11.00000 0.02597 0.01385 = 0.02185 -0.00416 -0.00643 0.00010 C13 1 0.637633 0.144851 0.471466 11.00000 0.02261 0.01890 = 0.02786 -0.00854 -0.00661 -0.00094 C14 1 0.712483 0.043972 0.500473 11.00000 0.02410 0.02292 = 0.02798 -0.00453 -0.00896 -0.00338 AFIX 43 H14 2 0.667461 -0.003674 0.556973 11.00000 -1.20000 AFIX 0 C15 1 0.853244 0.013666 0.446206 11.00000 0.02445 0.02550 = 0.03916 -0.01037 -0.01343 0.00230 AFIX 43 H15 2 0.903966 -0.055418 0.465123 11.00000 -1.20000 AFIX 0 C16 1 0.919851 0.083980 0.364533 11.00000 0.01848 0.03370 = 0.03996 -0.01347 -0.00210 -0.00237 AFIX 43 H16 2 1.016406 0.063457 0.327647 11.00000 -1.20000 AFIX 0 C17 1 0.844962 0.184365 0.336917 11.00000 0.02484 0.03031 = 0.03535 -0.00550 -0.00024 -0.00841 AFIX 43 H17 2 0.890722 0.232307 0.280802 11.00000 -1.20000 AFIX 0 C18 1 0.703992 0.215852 0.390110 11.00000 0.02641 0.01637 = 0.03396 -0.00381 -0.00391 -0.00275 AFIX 43 H18 2 0.653712 0.285069 0.371034 11.00000 -1.20000 AFIX 0 C19 1 -0.028532 0.208001 0.827221 11.00000 0.01721 0.02225 = 0.01723 0.00157 -0.00538 -0.00008 C20 1 -0.073317 0.295193 0.879057 11.00000 0.03069 0.02435 = 0.02162 -0.00100 -0.00317 -0.00291 AFIX 43 H20 2 -0.047268 0.369011 0.850141 11.00000 -1.20000 AFIX 0 C21 1 -0.155541 0.275327 0.972442 11.00000 0.03346 0.03601 = 0.02389 -0.00519 -0.00257 0.00170 AFIX 43 H21 2 -0.185788 0.335564 1.007004 11.00000 -1.20000 AFIX 0 C22 1 -0.193756 0.168310 1.015543 11.00000 0.02464 0.04679 = 0.02009 0.00417 -0.00194 -0.00167 AFIX 43 H22 2 -0.250573 0.154887 1.079463 11.00000 -1.20000 AFIX 0 C23 1 -0.149137 0.081656 0.965454 11.00000 0.03746 0.03085 = 0.03101 0.01061 -0.00327 -0.01303 AFIX 43 H23 2 -0.174847 0.008006 0.995128 11.00000 -1.20000 AFIX 0 C24 1 -0.066626 0.100388 0.871647 11.00000 0.03702 0.02117 = 0.02886 0.00281 -0.00722 -0.00759 AFIX 43 H24 2 -0.036161 0.039585 0.837778 11.00000 -1.20000 AFIX 0 C25 1 0.314375 0.130451 0.748259 11.00000 0.02004 0.01928 = 0.01741 0.00141 -0.00235 -0.00191 C26 1 0.355098 0.178730 0.818334 11.00000 0.02813 0.02046 = 0.02156 -0.00180 -0.00457 -0.00293 AFIX 43 H26 2 0.311758 0.249822 0.830879 11.00000 -1.20000 AFIX 0 C27 1 0.459000 0.122694 0.869636 11.00000 0.03420 0.03510 = 0.02382 -0.00218 -0.01290 -0.00425 AFIX 43 H27 2 0.486433 0.155746 0.917329 11.00000 -1.20000 AFIX 0 C28 1 0.523182 0.018977 0.852006 11.00000 0.02776 0.03596 = 0.02825 0.00513 -0.01239 0.00165 AFIX 43 H28 2 0.595501 -0.018216 0.886778 11.00000 -1.20000 AFIX 0 C29 1 0.481821 -0.030224 0.783793 11.00000 0.02866 0.02097 = 0.02688 0.00553 -0.00637 0.00180 AFIX 43 H29 2 0.525144 -0.101534 0.771886 11.00000 -1.20000 AFIX 0 C30 1 0.376445 0.024883 0.732451 11.00000 0.02793 0.01912 = 0.02130 0.00210 -0.00749 -0.00309 AFIX 43 H30 2 0.346718 -0.009689 0.686400 11.00000 -1.20000 AFIX 0 MOLE 2 C31 1 0.236300 0.316711 0.107729 11.00000 0.04349 0.02861 = 0.02974 -0.00246 -0.00237 0.00718 AFIX 13 H31 2 0.220240 0.333191 0.174093 11.00000 -1.20000 AFIX 0 CL2 5 0.139947 0.422063 0.041879 11.00000 0.05635 0.03738 = 0.05094 0.00631 -0.01535 0.00891 CL3 5 0.158920 0.188260 0.113093 11.00000 0.04264 0.02866 = 0.09422 -0.00115 0.01371 -0.00029 CL4 5 0.434168 0.311375 0.058604 11.00000 0.03848 0.04324 = 0.04636 -0.01089 -0.00675 -0.00223 HKLF 4 REM 2010acc1121b in P-1 REM R1 = 0.0470 for 5912 Fo > 4sig(Fo) and 0.0590 for all 7002 data REM 370 parameters refined using 0 restraints END WGHT 0.0000 3.7675 REM Highest difference peak 0.520, deepest hole -0.672, 1-sigma level 0.083 Q1 1 0.1777 0.3842 0.0019 11.00000 0.05 0.52 Q2 1 0.2016 0.2031 0.1586 11.00000 0.05 0.51 Q3 1 0.1988 0.4442 0.0613 11.00000 0.05 0.40 Q4 1 -0.1573 0.3444 0.5882 11.00000 0.05 0.38 Q5 1 0.2333 0.2387 0.6381 11.00000 0.05 0.37 Q6 1 0.6461 0.1782 0.4249 11.00000 0.05 0.37 Q7 1 0.0892 0.3188 0.5061 11.00000 0.05 0.37 Q8 1 -0.2317 0.3340 0.7693 11.00000 0.05 0.36 Q9 1 0.1732 0.2474 0.5700 11.00000 0.05 0.36 Q10 1 -0.0846 0.3058 0.6400 11.00000 0.05 0.36 Q11 1 0.3698 0.2560 0.4596 11.00000 0.05 0.35 Q12 1 0.1989 0.1993 0.0584 11.00000 0.05 0.35 Q13 1 0.3003 0.2536 0.5663 11.00000 0.05 0.35 Q14 1 0.0382 0.3979 0.3611 11.00000 0.05 0.34 Q15 1 0.6705 0.0858 0.4711 11.00000 0.05 0.34 Q16 1 0.2246 0.1781 0.6426 11.00000 0.05 0.34 Q17 1 -0.0461 0.1575 0.8548 11.00000 0.05 0.33 Q18 1 0.1294 0.1904 0.7171 11.00000 0.05 0.33 Q19 1 -0.0318 0.4111 0.4821 11.00000 0.05 0.33 Q20 1 0.2493 0.1555 0.7220 11.00000 0.05 0.32 ; #===END data_2010acc1142_complex_9 _database_code_depnum_ccdc_archive 'CCDC 817766' #TrackingRef '- Ogden_Dalton_combined.cif.txt' _chemical_compound_source 'Massimiliano Massi' _database_code_CSD 10AC1142 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H44 Co N6 S4, C2 H6 Cl3 Co O, C H Cl3' _chemical_formula_sum 'C63 H51 Cl6 Co2 N6 O S4' _chemical_formula_weight 1366.90 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' N N 0.0061 0.0033 '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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.8652(3) _cell_length_b 20.1328(3) _cell_length_c 18.0402(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.8240(10) _cell_angle_gamma 90.00 _cell_volume 6141.58(17) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 130226 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour 'Pale Brown' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2796 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8274 _exptl_absorpt_correction_T_max 0.9902 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64380 _diffrn_reflns_av_R_equivalents 0.1061 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10813 _reflns_number_gt 7911 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Images generated using CrystalMaker: a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd, Oxford, England (www.crystalmaker.com) ; _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+40.7849P] 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 10813 _refine_ls_number_parameters 744 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.1528 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _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 Co1 Co 0.24875(4) 0.51719(4) 0.64536(5) 0.01782(19) Uani 1 1 d . . . S1 S 0.30102(8) 0.47881(8) 0.77081(9) 0.0218(3) Uani 1 1 d . . . S2 S 0.22432(8) 0.56251(7) 0.52195(9) 0.0193(3) Uani 1 1 d . . . N1 N 0.4583(3) 0.4765(2) 0.8474(3) 0.0221(11) Uani 1 1 d . . . H901 H 0.5053 0.4882 0.8461 0.026 Uiso 1 1 calc R . . N2 N 0.3539(3) 0.5390(2) 0.6580(3) 0.0178(10) Uani 1 1 d . . . N3 N 0.3419(3) 0.6118(2) 0.4742(3) 0.0226(11) Uani 1 1 d . . . H903 H 0.3931 0.6193 0.4877 0.027 Uiso 1 1 calc R . . C1 C 0.3999(4) 0.4495(4) 0.9508(4) 0.0319(16) Uani 1 1 d . . . H1 H 0.3552 0.4767 0.9268 0.038 Uiso 1 1 calc R . . C2 C 0.4072(4) 0.4165(4) 1.0202(4) 0.0393(18) Uani 1 1 d . . . H2 H 0.3663 0.4202 1.0429 0.047 Uiso 1 1 calc R . . C3 C 0.4727(4) 0.3787(3) 1.0566(4) 0.0368(17) Uani 1 1 d . . . H3 H 0.4769 0.3566 1.1043 0.044 Uiso 1 1 calc R . . C4 C 0.5327(5) 0.3725(4) 1.0239(4) 0.0412(18) Uani 1 1 d . . . H4 H 0.5781 0.3464 1.0489 0.049 Uiso 1 1 calc R . . C5 C 0.5254(4) 0.4046(4) 0.9546(4) 0.0358(17) Uani 1 1 d . . . H5 H 0.5665 0.4011 0.9320 0.043 Uiso 1 1 calc R . . C6 C 0.4585(4) 0.4421(3) 0.9174(4) 0.0242(14) Uani 1 1 d . . . C7 C 0.3985(3) 0.4934(3) 0.7846(3) 0.0212(13) Uani 1 1 d . . . C8 C 0.4175(3) 0.5252(3) 0.7223(3) 0.0201(13) Uani 1 1 d . . . C9 C 0.4868(3) 0.5453(3) 0.7064(3) 0.0200(13) Uani 1 1 d . . . C10 C 0.4634(3) 0.5727(3) 0.6308(3) 0.0180(12) Uani 1 1 d . . . C11 C 0.3794(3) 0.5674(3) 0.6026(3) 0.0183(13) Uani 1 1 d . . . C12 C 0.3192(3) 0.5828(3) 0.5296(3) 0.0181(12) Uani 1 1 d . . . C13 C 0.2984(3) 0.6330(3) 0.3966(3) 0.0195(13) Uani 1 1 d . . . C14 C 0.3214(3) 0.6932(3) 0.3732(4) 0.0271(15) Uani 1 1 d . . . H14 H 0.3612 0.7194 0.4089 0.032 Uiso 1 1 calc R . . C15 C 0.2854(4) 0.7146(3) 0.2966(4) 0.0311(16) Uani 1 1 d . . . H15 H 0.3013 0.7553 0.2794 0.037 Uiso 1 1 calc R . . C16 C 0.2268(3) 0.6772(3) 0.2457(4) 0.0265(14) Uani 1 1 d . . . H16 H 0.2013 0.6928 0.1939 0.032 Uiso 1 1 calc R . . C17 C 0.2048(4) 0.6172(3) 0.2692(4) 0.0286(15) Uani 1 1 d . . . H17 H 0.1651 0.5913 0.2331 0.034 Uiso 1 1 calc R . . C18 C 0.2405(3) 0.5943(3) 0.3456(4) 0.0229(13) Uani 1 1 d . . . H18 H 0.2253 0.5531 0.3620 0.028 Uiso 1 1 calc R . . C19 C 0.5708(3) 0.5455(3) 0.7599(3) 0.0199(13) Uani 1 1 d . . . C20 C 0.6125(3) 0.4875(3) 0.7872(4) 0.0272(14) Uani 1 1 d . . . H20 H 0.5868 0.4458 0.7735 0.033 Uiso 1 1 calc R . . C21 C 0.6909(4) 0.4895(4) 0.8344(4) 0.0320(16) Uani 1 1 d . . . H21 H 0.7184 0.4493 0.8529 0.038 Uiso 1 1 calc R . . C22 C 0.7289(4) 0.5492(4) 0.8543(4) 0.0314(16) Uani 1 1 d . . . H22 H 0.7828 0.5505 0.8864 0.038 Uiso 1 1 calc R . . C23 C 0.6883(3) 0.6077(3) 0.8274(4) 0.0263(14) Uani 1 1 d . . . H23 H 0.7147 0.6491 0.8410 0.032 Uiso 1 1 calc R . . C24 C 0.6103(3) 0.6063(3) 0.7813(4) 0.0266(14) Uani 1 1 d . . . H24 H 0.5828 0.6468 0.7639 0.032 Uiso 1 1 calc R . . C25 C 0.5164(3) 0.5985(3) 0.5891(3) 0.0191(13) Uani 1 1 d . . . C26 C 0.5688(3) 0.5556(3) 0.5706(4) 0.0240(14) Uani 1 1 d . . . H26 H 0.5710 0.5101 0.5852 0.029 Uiso 1 1 calc R . . C27 C 0.6179(4) 0.5795(3) 0.5310(4) 0.0298(16) Uani 1 1 d . . . H27 H 0.6531 0.5502 0.5176 0.036 Uiso 1 1 calc R . . C28 C 0.6157(4) 0.6462(3) 0.5107(4) 0.0298(15) Uani 1 1 d . . . H28 H 0.6506 0.6626 0.4848 0.036 Uiso 1 1 calc R . . C29 C 0.5640(4) 0.6881(3) 0.5276(4) 0.0295(15) Uani 1 1 d . . . H29 H 0.5612 0.7333 0.5119 0.035 Uiso 1 1 calc R . . C30 C 0.5147(3) 0.6645(3) 0.5683(4) 0.0240(14) Uani 1 1 d . . . H30 H 0.4798 0.6942 0.5818 0.029 Uiso 1 1 calc R . . S3 S 0.25601(8) 0.41331(7) 0.59663(9) 0.0204(3) Uani 1 1 d . . . S4 S 0.21227(8) 0.61532(7) 0.69190(9) 0.0209(3) Uani 1 1 d . . . N4 N 0.1345(3) 0.3279(2) 0.5554(3) 0.0225(11) Uani 1 1 d . . . H4A H 0.0862 0.3180 0.5544 0.027 Uiso 1 1 calc R . . N5 N 0.1455(3) 0.4916(2) 0.6361(3) 0.0175(10) Uani 1 1 d . . . N6 N 0.0687(3) 0.6295(2) 0.7119(3) 0.0210(11) Uani 1 1 d . . . H6 H 0.0253 0.6079 0.7103 0.025 Uiso 1 1 calc R . . C31 C 0.2449(4) 0.2518(3) 0.5705(4) 0.0281(15) Uani 1 1 d . . . H31 H 0.2684 0.2653 0.6234 0.034 Uiso 1 1 calc R . . C32 C 0.2808(4) 0.2039(3) 0.5372(4) 0.0378(17) Uani 1 1 d . . . H32 H 0.3293 0.1845 0.5682 0.045 Uiso 1 1 calc R . . C33 C 0.2479(4) 0.1846(3) 0.4615(4) 0.0379(18) Uani 1 1 d . . . H33 H 0.2733 0.1521 0.4397 0.046 Uiso 1 1 calc R . . C34 C 0.1772(4) 0.2123(3) 0.4164(4) 0.0345(16) Uani 1 1 d . . . H34 H 0.1542 0.1991 0.3633 0.041 Uiso 1 1 calc R . . C35 C 0.1396(4) 0.2592(3) 0.4479(4) 0.0308(15) Uani 1 1 d . . . H35 H 0.0904 0.2778 0.4174 0.037 Uiso 1 1 calc R . . C36 C 0.1754(3) 0.2786(3) 0.5251(4) 0.0217(13) Uani 1 1 d . . . C37 C 0.1623(3) 0.3871(3) 0.5849(3) 0.0183(12) Uani 1 1 d . . . C38 C 0.1111(3) 0.4322(3) 0.6072(3) 0.0170(12) Uani 1 1 d . . . C39 C 0.0341(3) 0.4302(3) 0.6139(3) 0.0168(12) Uani 1 1 d . . . C40 C 0.0231(3) 0.4901(3) 0.6470(3) 0.0186(12) Uani 1 1 d . . . C41 C 0.0931(3) 0.5272(3) 0.6594(3) 0.0176(12) Uani 1 1 d . . . C42 C 0.1205(3) 0.5926(3) 0.6889(3) 0.0206(13) Uani 1 1 d . . . C43 C 0.0703(3) 0.6963(3) 0.7383(3) 0.0211(13) Uani 1 1 d . . . C44 C 0.0191(4) 0.7109(3) 0.7800(4) 0.0292(15) Uani 1 1 d . . . H44 H -0.0114 0.6765 0.7921 0.035 Uiso 1 1 calc R . . C45 C 0.0127(4) 0.7749(3) 0.8038(4) 0.0364(17) Uani 1 1 d . . . H45 H -0.0220 0.7848 0.8327 0.044 Uiso 1 1 calc R . . C46 C 0.0574(4) 0.8256(3) 0.7853(4) 0.0340(17) Uani 1 1 d . . . H46 H 0.0530 0.8700 0.8011 0.041 Uiso 1 1 calc R . . C47 C 0.1076(4) 0.8105(3) 0.7444(4) 0.0300(15) Uani 1 1 d . . . H47 H 0.1380 0.8449 0.7319 0.036 Uiso 1 1 calc R . . C48 C 0.1153(3) 0.7461(3) 0.7207(4) 0.0240(14) Uani 1 1 d . . . H48 H 0.1508 0.7363 0.6928 0.029 Uiso 1 1 calc R . . C49 C -0.0231(3) 0.3740(3) 0.5905(3) 0.0183(12) Uani 1 1 d . . . C50 C -0.0475(3) 0.3476(3) 0.5157(3) 0.0227(13) Uani 1 1 d . . . H50 H -0.0289 0.3664 0.4766 0.027 Uiso 1 1 calc R . . C51 C -0.0992(3) 0.2938(3) 0.4972(4) 0.0288(15) Uani 1 1 d . . . H51 H -0.1152 0.2757 0.4459 0.035 Uiso 1 1 calc R . . C52 C -0.1269(3) 0.2668(3) 0.5533(4) 0.0287(15) Uani 1 1 d . . . H52 H -0.1620 0.2300 0.5407 0.034 Uiso 1 1 calc R . . C53 C -0.1041(4) 0.2932(3) 0.6279(4) 0.0277(15) Uani 1 1 d . . . H53 H -0.1240 0.2749 0.6663 0.033 Uiso 1 1 calc R . . C54 C -0.0520(3) 0.3465(3) 0.6469(4) 0.0216(13) Uani 1 1 d . . . H54 H -0.0359 0.3643 0.6984 0.026 Uiso 1 1 calc R . . C55 C -0.0473(3) 0.5161(3) 0.6660(3) 0.0181(12) Uani 1 1 d . . . C56 C -0.1050(3) 0.5517(3) 0.6099(4) 0.0225(13) Uani 1 1 d . . . H56 H -0.1032 0.5551 0.5580 0.027 Uiso 1 1 calc R . . C57 C -0.1651(3) 0.5820(3) 0.6299(4) 0.0274(15) Uani 1 1 d . . . H57 H -0.2046 0.6061 0.5913 0.033 Uiso 1 1 calc R . . C58 C -0.1688(4) 0.5780(3) 0.7047(4) 0.0309(16) Uani 1 1 d . . . H58 H -0.2098 0.5999 0.7182 0.037 Uiso 1 1 calc R . . C59 C -0.1123(4) 0.5417(3) 0.7598(4) 0.0318(16) Uani 1 1 d . . . H59 H -0.1147 0.5382 0.8114 0.038 Uiso 1 1 calc R . . C60 C -0.0521(3) 0.5105(3) 0.7410(3) 0.0233(13) Uani 1 1 d . . . H60 H -0.0140 0.4851 0.7794 0.028 Uiso 1 1 calc R . . Co2 Co -0.00754(5) 0.61394(5) 0.04727(5) 0.0296(2) Uani 1 1 d . . . Cl1 Cl 0.01737(10) 0.68060(9) 0.15182(10) 0.0341(4) Uani 1 1 d . . . Cl2 Cl 0.10804(10) 0.56368(9) 0.05499(11) 0.0399(4) Uani 1 1 d . . . Cl3 Cl -0.07562(11) 0.65479(8) -0.07011(10) 0.0381(4) Uani 1 1 d . . . O1 O -0.0699(3) 0.5391(2) 0.0730(3) 0.0357(11) Uani 1 1 d D . . H99 H -0.085(4) 0.502(2) 0.033(3) 0.036(19) Uiso 1 1 d D . . C62 C -0.1392(5) 0.5487(4) 0.0963(6) 0.056(2) Uani 1 1 d . . . H62A H -0.1798 0.5735 0.0551 0.067 Uiso 1 1 calc R . . H62B H -0.1252 0.5751 0.1452 0.067 Uiso 1 1 calc R . . C63 C -0.1719(6) 0.4820(5) 0.1093(6) 0.078(3) Uani 1 1 d . . . H63A H -0.1938 0.4591 0.0590 0.117 Uiso 1 1 calc R . . H63B H -0.2136 0.4886 0.1329 0.117 Uiso 1 1 calc R . . H63C H -0.1293 0.4551 0.1443 0.117 Uiso 1 1 calc R . . C61 C 0.3638(4) 0.7663(3) 0.7011(4) 0.0325(16) Uani 1 1 d . . . H61 H 0.4119 0.7900 0.6981 0.039 Uiso 1 1 calc R . . Cl4 Cl 0.39447(12) 0.69987(11) 0.76552(15) 0.0655(7) Uani 1 1 d . . . Cl5 Cl 0.30629(12) 0.82333(10) 0.73306(12) 0.0506(5) Uani 1 1 d . . . Cl6 Cl 0.31009(11) 0.73765(9) 0.60648(11) 0.0428(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0149(4) 0.0177(4) 0.0228(4) 0.0015(3) 0.0088(3) -0.0007(3) S1 0.0181(7) 0.0230(8) 0.0267(8) 0.0038(7) 0.0104(6) -0.0014(6) S2 0.0157(7) 0.0211(8) 0.0224(8) 0.0018(6) 0.0081(6) -0.0007(6) N1 0.018(2) 0.027(3) 0.025(3) 0.009(2) 0.012(2) 0.003(2) N2 0.014(2) 0.019(3) 0.024(3) 0.000(2) 0.010(2) 0.0000(19) N3 0.016(2) 0.027(3) 0.023(3) 0.004(2) 0.004(2) -0.004(2) C1 0.020(3) 0.047(4) 0.035(4) 0.005(3) 0.018(3) 0.008(3) C2 0.035(4) 0.059(5) 0.030(4) 0.004(4) 0.018(3) -0.009(4) C3 0.055(5) 0.035(4) 0.024(4) 0.001(3) 0.017(3) -0.012(4) C4 0.055(5) 0.037(4) 0.035(4) 0.009(3) 0.019(4) 0.022(4) C5 0.031(4) 0.049(5) 0.029(4) 0.006(3) 0.012(3) 0.014(3) C6 0.029(3) 0.018(3) 0.023(3) 0.002(3) 0.004(3) 0.000(3) C7 0.018(3) 0.021(3) 0.026(3) 0.001(3) 0.009(3) 0.004(2) C8 0.019(3) 0.015(3) 0.025(3) 0.000(3) 0.006(3) 0.002(2) C9 0.016(3) 0.020(3) 0.029(3) -0.002(3) 0.013(3) 0.000(2) C10 0.018(3) 0.018(3) 0.020(3) -0.002(2) 0.009(2) 0.001(2) C11 0.012(3) 0.018(3) 0.027(3) 0.000(3) 0.008(2) 0.002(2) C12 0.021(3) 0.011(3) 0.024(3) 0.001(2) 0.010(3) 0.000(2) C13 0.017(3) 0.023(3) 0.020(3) 0.000(3) 0.009(3) 0.005(2) C14 0.019(3) 0.031(4) 0.032(4) 0.007(3) 0.009(3) -0.007(3) C15 0.029(4) 0.027(4) 0.041(4) 0.011(3) 0.016(3) 0.000(3) C16 0.019(3) 0.039(4) 0.024(3) 0.007(3) 0.010(3) 0.001(3) C17 0.023(3) 0.037(4) 0.025(4) -0.004(3) 0.007(3) -0.001(3) C18 0.020(3) 0.023(3) 0.029(4) -0.002(3) 0.013(3) -0.001(3) C19 0.013(3) 0.032(3) 0.018(3) 0.002(3) 0.009(2) 0.008(3) C20 0.022(3) 0.031(4) 0.030(4) 0.007(3) 0.010(3) 0.003(3) C21 0.020(3) 0.043(4) 0.034(4) 0.013(3) 0.009(3) 0.008(3) C22 0.014(3) 0.058(5) 0.021(3) 0.007(3) 0.005(3) 0.001(3) C23 0.020(3) 0.034(4) 0.027(4) -0.005(3) 0.011(3) -0.010(3) C24 0.017(3) 0.036(4) 0.029(4) -0.005(3) 0.010(3) -0.007(3) C25 0.016(3) 0.026(3) 0.015(3) 0.000(2) 0.005(2) -0.004(2) C26 0.020(3) 0.022(3) 0.029(4) 0.000(3) 0.007(3) 0.001(3) C27 0.023(3) 0.028(4) 0.048(4) -0.003(3) 0.026(3) 0.001(3) C28 0.025(3) 0.035(4) 0.037(4) -0.001(3) 0.020(3) -0.001(3) C29 0.032(4) 0.021(3) 0.043(4) 0.007(3) 0.024(3) 0.001(3) C30 0.023(3) 0.025(3) 0.030(4) 0.000(3) 0.017(3) 0.003(3) S3 0.0175(7) 0.0192(8) 0.0286(8) -0.0001(6) 0.0132(6) 0.0004(6) S4 0.0187(7) 0.0187(8) 0.0273(8) -0.0028(6) 0.0103(6) -0.0025(6) N4 0.018(3) 0.022(3) 0.031(3) -0.001(2) 0.013(2) -0.002(2) N5 0.019(2) 0.019(3) 0.018(3) 0.003(2) 0.011(2) 0.004(2) N6 0.020(3) 0.019(3) 0.027(3) -0.003(2) 0.011(2) -0.002(2) C31 0.024(3) 0.028(4) 0.033(4) -0.008(3) 0.009(3) 0.003(3) C32 0.026(4) 0.032(4) 0.053(5) -0.006(3) 0.009(3) 0.002(3) C33 0.048(4) 0.027(4) 0.053(5) -0.011(3) 0.036(4) 0.000(3) C34 0.048(4) 0.028(4) 0.029(4) -0.006(3) 0.016(3) -0.005(3) C35 0.036(4) 0.028(4) 0.029(4) -0.003(3) 0.011(3) 0.001(3) C36 0.017(3) 0.025(3) 0.028(3) -0.004(3) 0.013(3) -0.001(3) C37 0.016(3) 0.017(3) 0.020(3) 0.005(2) 0.004(2) 0.000(2) C38 0.016(3) 0.015(3) 0.020(3) 0.002(2) 0.006(2) -0.001(2) C39 0.016(3) 0.019(3) 0.015(3) -0.002(2) 0.003(2) -0.004(2) C40 0.020(3) 0.021(3) 0.015(3) 0.005(2) 0.006(2) 0.005(2) C41 0.021(3) 0.016(3) 0.021(3) -0.003(2) 0.013(2) 0.002(2) C42 0.021(3) 0.021(3) 0.020(3) 0.002(3) 0.007(3) 0.006(3) C43 0.019(3) 0.022(3) 0.021(3) -0.008(3) 0.003(3) -0.001(3) C44 0.026(3) 0.024(4) 0.042(4) -0.008(3) 0.017(3) -0.004(3) C45 0.033(4) 0.037(4) 0.047(5) -0.010(3) 0.023(3) -0.001(3) C46 0.034(4) 0.020(3) 0.046(4) -0.016(3) 0.011(3) 0.005(3) C47 0.031(4) 0.017(3) 0.039(4) -0.002(3) 0.008(3) -0.008(3) C48 0.022(3) 0.023(3) 0.027(3) -0.003(3) 0.009(3) -0.001(3) C49 0.016(3) 0.018(3) 0.020(3) -0.003(2) 0.006(2) 0.003(2) C50 0.022(3) 0.026(3) 0.020(3) -0.002(3) 0.008(3) -0.002(3) C51 0.021(3) 0.022(3) 0.036(4) -0.011(3) 0.000(3) 0.004(3) C52 0.016(3) 0.021(3) 0.047(4) -0.004(3) 0.008(3) -0.003(3) C53 0.027(3) 0.024(3) 0.033(4) 0.007(3) 0.012(3) 0.000(3) C54 0.021(3) 0.023(3) 0.027(3) -0.006(3) 0.016(3) 0.000(3) C55 0.013(3) 0.015(3) 0.027(3) 0.001(3) 0.009(2) -0.003(2) C56 0.016(3) 0.022(3) 0.030(4) 0.000(3) 0.009(3) -0.005(3) C57 0.015(3) 0.026(3) 0.039(4) 0.005(3) 0.006(3) 0.000(3) C58 0.030(4) 0.020(3) 0.051(5) -0.009(3) 0.024(3) -0.001(3) C59 0.032(4) 0.039(4) 0.033(4) -0.008(3) 0.024(3) -0.005(3) C60 0.019(3) 0.031(3) 0.020(3) 0.000(3) 0.006(3) -0.002(3) Co2 0.0272(5) 0.0310(5) 0.0311(5) 0.0063(4) 0.0099(4) 0.0040(4) Cl1 0.0317(9) 0.0421(10) 0.0282(9) 0.0023(7) 0.0091(7) 0.0055(7) Cl2 0.0266(9) 0.0372(10) 0.0543(12) -0.0031(9) 0.0109(8) 0.0023(7) Cl3 0.0488(11) 0.0318(9) 0.0284(9) 0.0064(7) 0.0051(8) 0.0072(8) O1 0.031(3) 0.034(3) 0.045(3) 0.000(2) 0.017(2) -0.002(2) C62 0.042(5) 0.051(5) 0.088(7) -0.004(5) 0.040(5) 0.005(4) C63 0.067(6) 0.105(9) 0.075(7) 0.005(6) 0.043(6) -0.004(6) C61 0.025(3) 0.030(4) 0.040(4) -0.001(3) 0.007(3) -0.002(3) Cl4 0.0411(11) 0.0589(14) 0.0765(16) 0.0263(12) -0.0087(11) -0.0088(10) Cl5 0.0493(11) 0.0579(13) 0.0519(12) -0.0207(10) 0.0265(10) -0.0002(10) Cl6 0.0441(10) 0.0438(11) 0.0405(11) -0.0158(8) 0.0138(9) -0.0066(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N5 1.870(5) . ? Co1 N2 1.871(4) . ? Co1 S1 2.2863(17) . ? Co1 S3 2.2885(17) . ? Co1 S2 2.3134(17) . ? Co1 S4 2.3208(17) . ? S1 C7 1.704(6) . ? S2 C12 1.705(6) . ? N1 C7 1.327(7) . ? N1 C6 1.438(7) . ? N2 C11 1.350(7) . ? N2 C8 1.365(7) . ? N3 C12 1.329(7) . ? N3 C13 1.429(7) . ? C1 C6 1.376(8) . ? C1 C2 1.385(9) . ? C2 C3 1.373(10) . ? C3 C4 1.386(10) . ? C4 C5 1.376(9) . ? C5 C6 1.390(9) . ? C7 C8 1.427(8) . ? C8 C9 1.416(8) . ? C9 C10 1.404(8) . ? C9 C19 1.500(8) . ? C10 C11 1.426(8) . ? C10 C25 1.480(8) . ? C11 C12 1.440(8) . ? C13 C18 1.382(8) . ? C13 C14 1.389(8) . ? C14 C15 1.392(9) . ? C15 C16 1.373(9) . ? C16 C17 1.378(9) . ? C17 C18 1.397(9) . ? C19 C20 1.386(8) . ? C19 C24 1.404(9) . ? C20 C21 1.385(9) . ? C21 C22 1.370(10) . ? C22 C23 1.387(9) . ? C23 C24 1.374(8) . ? C25 C30 1.379(8) . ? C25 C26 1.391(8) . ? C26 C27 1.383(8) . ? C27 C28 1.390(9) . ? C28 C29 1.356(9) . ? C29 C30 1.399(8) . ? S3 C37 1.702(6) . ? S4 C42 1.686(6) . ? N4 C37 1.334(7) . ? N4 C36 1.441(7) . ? N5 C41 1.348(7) . ? N5 C38 1.369(7) . ? N6 C42 1.353(7) . ? N6 C43 1.425(7) . ? C31 C36 1.360(8) . ? C31 C32 1.395(9) . ? C32 C33 1.360(10) . ? C33 C34 1.381(10) . ? C34 C35 1.384(9) . ? C35 C36 1.388(9) . ? C37 C38 1.436(8) . ? C38 C39 1.420(8) . ? C39 C40 1.388(8) . ? C39 C49 1.491(8) . ? C40 C41 1.413(8) . ? C40 C55 1.499(8) . ? C41 C42 1.444(8) . ? C43 C48 1.384(8) . ? C43 C44 1.390(8) . ? C44 C45 1.376(9) . ? C45 C46 1.401(10) . ? C46 C47 1.367(9) . ? C47 C48 1.384(9) . ? C49 C50 1.384(8) . ? C49 C54 1.394(8) . ? C50 C51 1.391(8) . ? C51 C52 1.374(9) . ? C52 C53 1.380(9) . ? C53 C54 1.390(8) . ? C55 C60 1.387(8) . ? C55 C56 1.389(8) . ? C56 C57 1.380(8) . ? C57 C58 1.375(9) . ? C58 C59 1.375(10) . ? C59 C60 1.379(8) . ? Co2 O1 2.016(5) . ? Co2 Cl3 2.2310(19) . ? Co2 Cl1 2.2394(19) . ? Co2 Cl2 2.2632(19) . ? O1 C62 1.443(8) . ? C62 C63 1.512(12) . ? C61 Cl4 1.741(7) . ? C61 Cl5 1.756(7) . ? C61 Cl6 1.764(7) . ? 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 N5 Co1 N2 177.0(2) . . ? N5 Co1 S1 94.08(15) . . ? N2 Co1 S1 83.43(15) . . ? N5 Co1 S3 83.72(15) . . ? N2 Co1 S3 94.71(15) . . ? S1 Co1 S3 90.90(6) . . ? N5 Co1 S2 98.54(15) . . ? N2 Co1 S2 83.95(15) . . ? S1 Co1 S2 167.38(6) . . ? S3 Co1 S2 90.42(6) . . ? N5 Co1 S4 83.26(15) . . ? N2 Co1 S4 98.31(15) . . ? S1 Co1 S4 90.13(6) . . ? S3 Co1 S4 166.98(6) . . ? S2 Co1 S4 91.41(6) . . ? C7 S1 Co1 99.1(2) . . ? C12 S2 Co1 98.2(2) . . ? C7 N1 C6 130.3(5) . . ? C11 N2 C8 109.2(5) . . ? C11 N2 Co1 125.0(4) . . ? C8 N2 Co1 125.7(4) . . ? C12 N3 C13 131.7(5) . . ? C6 C1 C2 118.8(6) . . ? C3 C2 C1 121.1(6) . . ? C2 C3 C4 120.2(6) . . ? C5 C4 C3 119.1(7) . . ? C4 C5 C6 120.6(6) . . ? C1 C6 C5 120.3(6) . . ? C1 C6 N1 123.1(6) . . ? C5 C6 N1 116.4(6) . . ? N1 C7 C8 117.2(5) . . ? N1 C7 S1 125.7(5) . . ? C8 C7 S1 117.0(4) . . ? N2 C8 C9 108.1(5) . . ? N2 C8 C7 114.6(5) . . ? C9 C8 C7 137.2(5) . . ? C10 C9 C8 107.7(5) . . ? C10 C9 C19 123.1(5) . . ? C8 C9 C19 129.0(5) . . ? C9 C10 C11 105.4(5) . . ? C9 C10 C25 126.4(5) . . ? C11 C10 C25 128.1(5) . . ? N2 C11 C10 109.6(5) . . ? N2 C11 C12 116.0(5) . . ? C10 C11 C12 134.4(5) . . ? N3 C12 C11 117.6(5) . . ? N3 C12 S2 125.5(5) . . ? C11 C12 S2 116.8(4) . . ? C18 C13 C14 121.3(6) . . ? C18 C13 N3 122.5(5) . . ? C14 C13 N3 116.0(5) . . ? C13 C14 C15 119.1(6) . . ? C16 C15 C14 120.1(6) . . ? C15 C16 C17 120.4(6) . . ? C16 C17 C18 120.6(6) . . ? C13 C18 C17 118.4(6) . . ? C20 C19 C24 118.2(5) . . ? C20 C19 C9 122.5(6) . . ? C24 C19 C9 119.3(5) . . ? C21 C20 C19 120.9(6) . . ? C22 C21 C20 120.3(6) . . ? C21 C22 C23 119.6(6) . . ? C24 C23 C22 120.5(6) . . ? C23 C24 C19 120.4(6) . . ? C30 C25 C26 119.4(5) . . ? C30 C25 C10 120.9(5) . . ? C26 C25 C10 119.7(5) . . ? C27 C26 C25 119.7(6) . . ? C26 C27 C28 120.3(6) . . ? C29 C28 C27 120.2(6) . . ? C28 C29 C30 119.9(6) . . ? C25 C30 C29 120.4(6) . . ? C37 S3 Co1 98.9(2) . . ? C42 S4 Co1 98.1(2) . . ? C37 N4 C36 126.7(5) . . ? C41 N5 C38 108.2(5) . . ? C41 N5 Co1 126.1(4) . . ? C38 N5 Co1 125.7(4) . . ? C42 N6 C43 132.7(5) . . ? C36 C31 C32 118.2(6) . . ? C33 C32 C31 121.4(7) . . ? C32 C33 C34 119.5(6) . . ? C33 C34 C35 120.5(6) . . ? C34 C35 C36 118.4(6) . . ? C31 C36 C35 121.9(6) . . ? C31 C36 N4 121.4(5) . . ? C35 C36 N4 116.7(5) . . ? N4 C37 C38 119.2(5) . . ? N4 C37 S3 123.5(4) . . ? C38 C37 S3 117.4(4) . . ? N5 C38 C39 108.7(5) . . ? N5 C38 C37 114.2(5) . . ? C39 C38 C37 136.8(5) . . ? C40 C39 C38 106.7(5) . . ? C40 C39 C49 127.0(5) . . ? C38 C39 C49 126.3(5) . . ? C39 C40 C41 106.6(5) . . ? C39 C40 C55 130.3(5) . . ? C41 C40 C55 123.0(5) . . ? N5 C41 C40 109.7(5) . . ? N5 C41 C42 114.4(5) . . ? C40 C41 C42 135.9(5) . . ? N6 C42 C41 115.4(5) . . ? N6 C42 S4 126.6(5) . . ? C41 C42 S4 118.0(4) . . ? C48 C43 C44 120.2(6) . . ? C48 C43 N6 123.9(5) . . ? C44 C43 N6 115.7(5) . . ? C45 C44 C43 120.1(6) . . ? C44 C45 C46 119.7(6) . . ? C47 C46 C45 119.4(6) . . ? C46 C47 C48 121.5(6) . . ? C47 C48 C43 119.0(6) . . ? C50 C49 C54 119.1(5) . . ? C50 C49 C39 122.5(5) . . ? C54 C49 C39 118.4(5) . . ? C49 C50 C51 120.5(6) . . ? C52 C51 C50 120.1(6) . . ? C51 C52 C53 120.1(6) . . ? C52 C53 C54 120.1(6) . . ? C53 C54 C49 120.1(6) . . ? C60 C55 C56 119.1(5) . . ? C60 C55 C40 121.0(5) . . ? C56 C55 C40 119.6(5) . . ? C57 C56 C55 119.7(6) . . ? C58 C57 C56 121.3(6) . . ? C57 C58 C59 118.9(6) . . ? C58 C59 C60 120.9(6) . . ? C59 C60 C55 120.1(6) . . ? O1 Co2 Cl3 108.77(15) . . ? O1 Co2 Cl1 103.20(15) . . ? Cl3 Co2 Cl1 118.54(7) . . ? O1 Co2 Cl2 102.29(14) . . ? Cl3 Co2 Cl2 115.49(8) . . ? Cl1 Co2 Cl2 106.66(7) . . ? C62 O1 Co2 123.8(4) . . ? O1 C62 C63 109.6(7) . . ? Cl4 C61 Cl5 112.0(4) . . ? Cl4 C61 Cl6 110.5(4) . . ? Cl5 C61 Cl6 109.8(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H99 Cl2 1.02(2) 2.00(2) 3.010(5) 172(6) 3_565 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.037 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.113 _iucr_refine_instruction_details ; TITL 2010acc1142 in P2(1)/n CELL 0.71073 17.8652 20.1328 18.0402 90.000 108.824 90.000 ZERR 4.00 0.0003 0.0003 0.0003 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N S CL CO O UNIT 252 204 24 16 24 8 4 MERG 2 SHEL 7 0.84 HTAB O1 Cl2_$1 EQIV $1 [ -x, -y+1, -z ] FMAP 2 PLAN 10 SIZE 0.01 0.07 0.20 DFIX 1.0 O1 H99 ACTA 55.00 BOND L.S. 4 TEMP -153.00 WGHT 0.000000 40.784908 FVAR 0.26364 CO1 6 0.248749 0.517190 0.645355 11.00000 0.01488 0.01772 = 0.02278 0.00151 0.00876 -0.00068 MOLE 1 S1 4 0.301018 0.478812 0.770809 11.00000 0.01805 0.02302 = 0.02672 0.00378 0.01044 -0.00137 S2 4 0.224319 0.562512 0.521955 11.00000 0.01571 0.02109 = 0.02245 0.00180 0.00807 -0.00069 N1 3 0.458318 0.476494 0.847418 11.00000 0.01821 0.02742 = 0.02453 0.00936 0.01234 0.00310 AFIX 43 H901 2 0.505326 0.488180 0.846070 11.00000 -1.20000 AFIX 0 N2 3 0.353949 0.539009 0.657967 11.00000 0.01374 0.01872 = 0.02422 -0.00047 0.01048 0.00004 N3 3 0.341921 0.611796 0.474164 11.00000 0.01595 0.02696 = 0.02302 0.00367 0.00355 -0.00415 AFIX 43 H903 2 0.393103 0.619292 0.487698 11.00000 -1.20000 AFIX 0 C1 1 0.399921 0.449504 0.950839 11.00000 0.02047 0.04664 = 0.03516 0.00465 0.01790 0.00834 AFIX 43 H1 2 0.355232 0.476737 0.926826 11.00000 -1.20000 AFIX 0 C2 1 0.407219 0.416526 1.020177 11.00000 0.03466 0.05866 = 0.02993 0.00410 0.01779 -0.00926 AFIX 43 H2 2 0.366270 0.420164 1.042915 11.00000 -1.20000 AFIX 0 C3 1 0.472685 0.378654 1.056597 11.00000 0.05513 0.03466 = 0.02355 0.00083 0.01657 -0.01207 AFIX 43 H3 2 0.476873 0.356633 1.104343 11.00000 -1.20000 AFIX 0 C4 1 0.532665 0.372472 1.023879 11.00000 0.05501 0.03678 = 0.03507 0.00939 0.01918 0.02175 AFIX 43 H4 2 0.578146 0.346425 1.048935 11.00000 -1.20000 AFIX 0 C5 1 0.525414 0.404591 0.954600 11.00000 0.03109 0.04877 = 0.02908 0.00560 0.01172 0.01394 AFIX 43 H5 2 0.566490 0.401086 0.932013 11.00000 -1.20000 AFIX 0 C6 1 0.458548 0.442120 0.917351 11.00000 0.02893 0.01770 = 0.02298 0.00231 0.00429 0.00029 C7 1 0.398524 0.493399 0.784600 11.00000 0.01767 0.02065 = 0.02648 0.00123 0.00879 0.00380 C8 1 0.417526 0.525213 0.722295 11.00000 0.01861 0.01547 = 0.02522 -0.00031 0.00581 0.00168 C9 1 0.486803 0.545250 0.706377 11.00000 0.01574 0.01987 = 0.02875 -0.00219 0.01338 0.00013 C10 1 0.463432 0.572730 0.630806 11.00000 0.01784 0.01806 = 0.02031 -0.00188 0.00933 0.00142 C11 1 0.379365 0.567358 0.602584 11.00000 0.01167 0.01808 = 0.02650 -0.00003 0.00819 0.00212 C12 1 0.319197 0.582821 0.529589 11.00000 0.02116 0.01117 = 0.02420 0.00128 0.01043 -0.00041 C13 1 0.298415 0.632987 0.396634 11.00000 0.01711 0.02322 = 0.02039 -0.00025 0.00904 0.00485 C14 1 0.321422 0.693189 0.373181 11.00000 0.01900 0.03053 = 0.03193 0.00730 0.00861 -0.00701 AFIX 43 H14 2 0.361198 0.719350 0.408926 11.00000 -1.20000 AFIX 0 C15 1 0.285368 0.714647 0.296554 11.00000 0.02868 0.02705 = 0.04081 0.01113 0.01574 0.00026 AFIX 43 H15 2 0.301309 0.755279 0.279431 11.00000 -1.20000 AFIX 0 C16 1 0.226826 0.677217 0.245679 11.00000 0.01889 0.03911 = 0.02355 0.00747 0.00973 0.00066 AFIX 43 H16 2 0.201297 0.692761 0.193938 11.00000 -1.20000 AFIX 0 C17 1 0.204847 0.617244 0.269170 11.00000 0.02310 0.03657 = 0.02548 -0.00372 0.00684 -0.00094 AFIX 43 H17 2 0.165115 0.591274 0.233105 11.00000 -1.20000 AFIX 0 C18 1 0.240499 0.594302 0.345577 11.00000 0.02044 0.02257 = 0.02913 -0.00180 0.01265 -0.00052 AFIX 43 H18 2 0.225291 0.553092 0.362044 11.00000 -1.20000 AFIX 0 C19 1 0.570837 0.545472 0.759887 11.00000 0.01300 0.03164 = 0.01817 0.00226 0.00943 0.00763 C20 1 0.612455 0.487524 0.787230 11.00000 0.02169 0.03084 = 0.02992 0.00707 0.00967 0.00309 AFIX 43 H20 2 0.586830 0.445831 0.773454 11.00000 -1.20000 AFIX 0 C21 1 0.690876 0.489522 0.834355 11.00000 0.01956 0.04257 = 0.03422 0.01306 0.00910 0.00842 AFIX 43 H21 2 0.718417 0.449335 0.852916 11.00000 -1.20000 AFIX 0 C22 1 0.728890 0.549194 0.854311 11.00000 0.01424 0.05783 = 0.02121 0.00677 0.00455 0.00140 AFIX 43 H22 2 0.782764 0.550470 0.886392 11.00000 -1.20000 AFIX 0 C23 1 0.688305 0.607727 0.827430 11.00000 0.01979 0.03423 = 0.02736 -0.00547 0.01090 -0.01024 AFIX 43 H23 2 0.714671 0.649140 0.840992 11.00000 -1.20000 AFIX 0 C24 1 0.610272 0.606318 0.781342 11.00000 0.01659 0.03590 = 0.02885 -0.00495 0.00963 -0.00665 AFIX 43 H24 2 0.582841 0.646755 0.763891 11.00000 -1.20000 AFIX 0 C25 1 0.516403 0.598469 0.589051 11.00000 0.01609 0.02568 = 0.01542 0.00029 0.00490 -0.00444 C26 1 0.568850 0.555616 0.570612 11.00000 0.01974 0.02250 = 0.02943 -0.00002 0.00732 0.00065 AFIX 43 H26 2 0.571000 0.510130 0.585163 11.00000 -1.20000 AFIX 0 C27 1 0.617861 0.579514 0.530998 11.00000 0.02308 0.02812 = 0.04826 -0.00310 0.02563 0.00072 AFIX 43 H27 2 0.653148 0.550181 0.517625 11.00000 -1.20000 AFIX 0 C28 1 0.615737 0.646238 0.510661 11.00000 0.02462 0.03503 = 0.03718 -0.00132 0.02045 -0.00058 AFIX 43 H28 2 0.650637 0.662607 0.484810 11.00000 -1.20000 AFIX 0 C29 1 0.563976 0.688056 0.527615 11.00000 0.03220 0.02113 = 0.04330 0.00724 0.02354 0.00110 AFIX 43 H29 2 0.561206 0.733263 0.511862 11.00000 -1.20000 AFIX 0 C30 1 0.514693 0.664530 0.568318 11.00000 0.02314 0.02539 = 0.02979 0.00016 0.01740 0.00293 AFIX 43 H30 2 0.479816 0.694239 0.581771 11.00000 -1.20000 AFIX 0 MOLE 2 S3 4 0.256013 0.413306 0.596634 11.00000 0.01750 0.01922 = 0.02863 -0.00005 0.01320 0.00038 S4 4 0.212270 0.615320 0.691899 11.00000 0.01868 0.01870 = 0.02730 -0.00279 0.01030 -0.00245 N4 3 0.134516 0.327914 0.555417 11.00000 0.01824 0.02209 = 0.03062 -0.00090 0.01286 -0.00249 AFIX 43 H4A 2 0.086231 0.317956 0.554399 11.00000 -1.20000 AFIX 0 N5 3 0.145485 0.491602 0.636116 11.00000 0.01888 0.01873 = 0.01818 0.00306 0.01068 0.00388 N6 3 0.068661 0.629489 0.711921 11.00000 0.01986 0.01902 = 0.02698 -0.00303 0.01143 -0.00238 AFIX 43 H6 2 0.025321 0.607908 0.710283 11.00000 -1.20000 AFIX 0 C31 1 0.244913 0.251781 0.570470 11.00000 0.02389 0.02769 = 0.03272 -0.00815 0.00907 0.00324 AFIX 43 H31 2 0.268416 0.265265 0.623382 11.00000 -1.20000 AFIX 0 C32 1 0.280823 0.203941 0.537247 11.00000 0.02561 0.03246 = 0.05274 -0.00632 0.00923 0.00183 AFIX 43 H32 2 0.329282 0.184513 0.568217 11.00000 -1.20000 AFIX 0 C33 1 0.247896 0.184554 0.461466 11.00000 0.04845 0.02659 = 0.05268 -0.01086 0.03562 0.00017 AFIX 43 H33 2 0.273350 0.152127 0.439695 11.00000 -1.20000 AFIX 0 C34 1 0.177210 0.212322 0.416373 11.00000 0.04836 0.02826 = 0.02941 -0.00607 0.01604 -0.00456 AFIX 43 H34 2 0.154228 0.199104 0.363298 11.00000 -1.20000 AFIX 0 C35 1 0.139585 0.259249 0.447883 11.00000 0.03563 0.02831 = 0.02927 -0.00304 0.01143 0.00128 AFIX 43 H35 2 0.090396 0.277801 0.417379 11.00000 -1.20000 AFIX 0 C36 1 0.175381 0.278580 0.525081 11.00000 0.01664 0.02522 = 0.02761 -0.00369 0.01334 -0.00140 C37 1 0.162326 0.387124 0.584886 11.00000 0.01644 0.01711 = 0.02017 0.00518 0.00413 -0.00014 C38 1 0.111073 0.432196 0.607211 11.00000 0.01639 0.01501 = 0.01977 0.00209 0.00595 -0.00062 C39 1 0.034066 0.430164 0.613890 11.00000 0.01562 0.01882 = 0.01503 -0.00157 0.00350 -0.00401 C40 1 0.023063 0.490073 0.647035 11.00000 0.01966 0.02128 = 0.01523 0.00466 0.00599 0.00528 C41 1 0.093144 0.527221 0.659391 11.00000 0.02062 0.01571 = 0.02079 -0.00292 0.01271 0.00185 C42 1 0.120505 0.592601 0.688851 11.00000 0.02056 0.02103 = 0.02047 0.00175 0.00702 0.00581 C43 1 0.070328 0.696341 0.738339 11.00000 0.01853 0.02204 = 0.02079 -0.00820 0.00349 -0.00074 C44 1 0.019144 0.710864 0.780030 11.00000 0.02582 0.02435 = 0.04200 -0.00805 0.01719 -0.00401 AFIX 43 H44 2 -0.011447 0.676482 0.792134 11.00000 -1.20000 AFIX 0 C45 1 0.012675 0.774923 0.803816 11.00000 0.03283 0.03654 = 0.04714 -0.01007 0.02298 -0.00110 AFIX 43 H45 2 -0.022022 0.784778 0.832660 11.00000 -1.20000 AFIX 0 C46 1 0.057449 0.825562 0.785339 11.00000 0.03413 0.01968 = 0.04640 -0.01633 0.01051 0.00460 AFIX 43 H46 2 0.052971 0.870000 0.801112 11.00000 -1.20000 AFIX 0 C47 1 0.107650 0.810468 0.744406 11.00000 0.03136 0.01741 = 0.03869 -0.00224 0.00792 -0.00758 AFIX 43 H47 2 0.137960 0.844889 0.731950 11.00000 -1.20000 AFIX 0 C48 1 0.115288 0.746150 0.720715 11.00000 0.02233 0.02350 = 0.02731 -0.00283 0.00949 -0.00090 AFIX 43 H48 2 0.150833 0.736334 0.692791 11.00000 -1.20000 AFIX 0 C49 1 -0.023121 0.373987 0.590537 11.00000 0.01640 0.01845 = 0.02040 -0.00262 0.00634 0.00305 C50 1 -0.047548 0.347645 0.515661 11.00000 0.02243 0.02592 = 0.02045 -0.00201 0.00781 -0.00209 AFIX 43 H50 2 -0.028944 0.366438 0.476560 11.00000 -1.20000 AFIX 0 C51 1 -0.099154 0.293838 0.497243 11.00000 0.02112 0.02238 = 0.03638 -0.01090 0.00000 0.00361 AFIX 43 H51 2 -0.115191 0.275741 0.445867 11.00000 -1.20000 AFIX 0 C52 1 -0.126948 0.266850 0.553313 11.00000 0.01649 0.02133 = 0.04677 -0.00403 0.00818 -0.00338 AFIX 43 H52 2 -0.161958 0.229968 0.540703 11.00000 -1.20000 AFIX 0 C53 1 -0.104099 0.293222 0.627878 11.00000 0.02706 0.02428 = 0.03318 0.00670 0.01163 0.00006 AFIX 43 H53 2 -0.124045 0.274899 0.666286 11.00000 -1.20000 AFIX 0 C54 1 -0.051963 0.346535 0.646901 11.00000 0.02103 0.02262 = 0.02711 -0.00553 0.01595 -0.00042 AFIX 43 H54 2 -0.035943 0.364311 0.698432 11.00000 -1.20000 AFIX 0 C55 1 -0.047270 0.516057 0.666012 11.00000 0.01336 0.01543 = 0.02738 0.00087 0.00934 -0.00342 C56 1 -0.105012 0.551661 0.609932 11.00000 0.01642 0.02199 = 0.03012 -0.00017 0.00886 -0.00500 AFIX 43 H56 2 -0.103180 0.555125 0.558027 11.00000 -1.20000 AFIX 0 C57 1 -0.165057 0.581985 0.629933 11.00000 0.01510 0.02618 = 0.03876 0.00465 0.00557 -0.00018 AFIX 43 H57 2 -0.204564 0.606097 0.591278 11.00000 -1.20000 AFIX 0 C58 1 -0.168823 0.577980 0.704732 11.00000 0.03029 0.02008 = 0.05056 -0.00853 0.02446 -0.00143 AFIX 43 H58 2 -0.209769 0.599874 0.718163 11.00000 -1.20000 AFIX 0 C59 1 -0.112301 0.541739 0.759756 11.00000 0.03244 0.03900 = 0.03342 -0.00834 0.02356 -0.00468 AFIX 43 H59 2 -0.114730 0.538190 0.811442 11.00000 -1.20000 AFIX 0 C60 1 -0.052129 0.510469 0.740965 11.00000 0.01903 0.03125 = 0.01964 -0.00033 0.00620 -0.00246 AFIX 43 H60 2 -0.013952 0.485065 0.779408 11.00000 -1.20000 AFIX 0 MOLE 3 CO2 6 -0.007544 0.613942 0.047272 11.00000 0.02718 0.03102 = 0.03112 0.00634 0.00994 0.00397 CL1 5 0.017365 0.680604 0.151819 11.00000 0.03168 0.04206 = 0.02819 0.00227 0.00908 0.00545 CL2 5 0.108040 0.563677 0.054990 11.00000 0.02661 0.03718 = 0.05427 -0.00307 0.01094 0.00232 CL3 5 -0.075615 0.654792 -0.070106 11.00000 0.04877 0.03178 = 0.02842 0.00640 0.00508 0.00719 O1 7 -0.069935 0.539067 0.073028 11.00000 0.03143 0.03362 = 0.04534 -0.00020 0.01708 -0.00172 H99 2 -0.085111 0.501866 0.032867 11.00000 0.03618 C62 1 -0.139209 0.548726 0.096315 11.00000 0.04187 0.05143 = 0.08780 -0.00440 0.04017 0.00468 AFIX 23 H62A 2 -0.179798 0.573487 0.055053 11.00000 -1.20000 H62B 2 -0.125218 0.575116 0.145195 11.00000 -1.20000 AFIX 0 C63 1 -0.171864 0.482029 0.109282 11.00000 0.06722 0.10529 = 0.07547 0.00503 0.04306 -0.00352 AFIX 137 H63A 2 -0.193823 0.459145 0.058963 11.00000 -1.50000 H63B 2 -0.213585 0.488589 0.132938 11.00000 -1.50000 H63C 2 -0.129349 0.455126 0.144348 11.00000 -1.50000 AFIX 0 MOLE 4 C61 1 0.363771 0.766333 0.701129 11.00000 0.02540 0.03024 = 0.03962 -0.00110 0.00749 -0.00192 AFIX 13 H61 2 0.411917 0.789980 0.698085 11.00000 -1.20000 AFIX 0 CL4 5 0.394466 0.699866 0.765524 11.00000 0.04107 0.05891 = 0.07649 0.02629 -0.00867 -0.00878 CL5 5 0.306286 0.823326 0.733061 11.00000 0.04926 0.05789 = 0.05189 -0.02073 0.02646 -0.00016 CL6 5 0.310091 0.737647 0.606480 11.00000 0.04408 0.04378 = 0.04051 -0.01576 0.01381 -0.00662 HKLF 4 REM 2010acc1142 in P2(1)/n REM R1 = 0.0776 for 7911 Fo > 4sig(Fo) and 0.1155 for all 10813 data REM 744 parameters refined using 1 restraints END WGHT 0.0000 40.7219 REM Highest difference peak 1.037, deepest hole -0.601, 1-sigma level 0.113 Q1 1 -0.2019 0.5791 0.0620 11.00000 0.05 1.04 Q2 1 -0.0231 0.5773 0.0046 11.00000 0.05 0.80 Q3 1 0.1030 0.5778 0.0009 11.00000 0.05 0.52 Q4 1 0.0316 0.6397 0.1191 11.00000 0.05 0.50 Q5 1 0.6039 0.3578 1.0731 11.00000 0.05 0.49 Q6 1 0.1826 0.4981 0.6160 11.00000 0.05 0.44 Q7 1 0.5841 0.4455 1.0551 11.00000 0.05 0.44 Q8 1 0.2427 0.5574 0.5773 11.00000 0.05 0.43 Q9 1 -0.0156 0.4964 0.6531 11.00000 0.05 0.43 Q10 1 -0.0964 0.4633 0.0008 11.00000 0.05 0.42 ; #===END