Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Maravanji Balakrishna' 'Joel Mague' 'Dulal Panda' 'Krishnan Rathinasamy' D.Suresh _publ_contact_author_name 'Maravanji Balakrishna' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Bombay Powai Mumbai 400076 INDIA ; _publ_contact_author_email KRISHNA@CHEM.IITB.AC.IN _publ_section_title ; Large Bite Bis(phosphite) Ligand Containing Mesocyclic Thioether Moieties: Synthesis, Reactivity, Group 11 (CuI, AuI) Metal Complexes and Anticancer Activity Studies on Human Cervical Cancer (HeLa) Cell Line ; # Attachment 'msb303.cif' data_msb303 _database_code_depnum_ccdc_archive 'CCDC 672312' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H39 Cu I N O6 P2 S3' _chemical_formula_sum 'C62 H39 Cu I N O6 P2 S3' _chemical_formula_weight 1242.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 14.799(1) _cell_length_b 16.396(1) _cell_length_c 22.002(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.064(1) _cell_angle_gamma 90.00 _cell_volume 5178.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9275 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.29 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 1.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8377 _exptl_absorpt_correction_T_max 0.9261 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90166 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 28.34 _reflns_number_total 12898 _reflns_number_gt 10214 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _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^)+(0.0413P)^2^+5.7705P] 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 12898 _refine_ls_number_parameters 686 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 I I 0.413787(13) 0.326042(13) 0.122696(9) 0.01915(6) Uani 1 1 d . . . Cu Cu 0.24298(2) 0.30345(2) 0.083340(16) 0.01297(8) Uani 1 1 d . . . S1 S 0.29301(5) 0.23550(4) -0.03406(3) 0.01343(14) Uani 1 1 d . . . S2 S -0.07597(5) 0.35542(4) 0.06594(3) 0.01468(15) Uani 1 1 d . . . S3 S 0.25996(5) 0.10281(4) 0.09558(3) 0.01434(15) Uani 1 1 d . . . P1 P 0.15215(5) 0.34475(5) -0.00668(3) 0.01213(15) Uani 1 1 d . . . P2 P 0.15659(5) 0.23862(5) 0.13673(3) 0.01238(15) Uani 1 1 d . . . O1 O 0.08940(13) 0.27837(12) -0.05198(9) 0.0144(4) Uani 1 1 d . . . O2 O 0.18996(14) 0.39861(12) -0.05730(9) 0.0154(4) Uani 1 1 d . . . O3 O 0.06330(13) 0.39911(12) -0.00149(9) 0.0143(4) Uani 1 1 d . . . O4 O 0.09453(13) 0.30347(12) 0.16340(9) 0.0140(4) Uani 1 1 d . . . O5 O 0.19519(14) 0.18430(12) 0.19958(9) 0.0146(4) Uani 1 1 d . . . O6 O 0.07572(13) 0.17873(12) 0.09852(9) 0.0136(4) Uani 1 1 d . . . C1 C 0.1120(2) 0.23618(17) -0.10046(13) 0.0137(6) Uani 1 1 d . . . C2 C 0.2014(2) 0.21384(18) -0.10059(13) 0.0141(6) Uani 1 1 d . . . C3 C 0.2176(2) 0.16495(18) -0.15113(14) 0.0151(6) Uani 1 1 d . . . C4 C 0.3079(2) 0.13879(19) -0.15433(15) 0.0191(6) Uani 1 1 d . . . H4 H 0.3608 0.1542 -0.1224 0.023 Uiso 1 1 calc R . . C5 C 0.3190(2) 0.0916(2) -0.20305(15) 0.0230(7) Uani 1 1 d . . . H5 H 0.3799 0.0753 -0.2050 0.028 Uiso 1 1 calc R . . C6 C 0.2420(2) 0.0667(2) -0.25042(15) 0.0227(7) Uani 1 1 d . . . H6 H 0.2508 0.0328 -0.2835 0.027 Uiso 1 1 calc R . . C7 C 0.1550(2) 0.0911(2) -0.24874(15) 0.0214(7) Uani 1 1 d . . . H7 H 0.1033 0.0743 -0.2811 0.026 Uiso 1 1 calc R . . C8 C 0.1399(2) 0.14148(18) -0.19949(14) 0.0169(6) Uani 1 1 d . . . C9 C 0.0497(2) 0.16753(18) -0.19751(14) 0.0172(6) Uani 1 1 d . . . H9 H -0.0021 0.1524 -0.2304 0.021 Uiso 1 1 calc R . . C10 C 0.0357(2) 0.21410(18) -0.14924(14) 0.0161(6) Uani 1 1 d . . . H10 H -0.0253 0.2315 -0.1486 0.019 Uiso 1 1 calc R . . C11 C 0.2822(2) 0.39946(18) -0.06131(13) 0.0151(6) Uani 1 1 d . . . C12 C 0.3368(2) 0.33105(18) -0.05376(13) 0.0141(6) Uani 1 1 d . . . C13 C 0.4323(2) 0.33775(19) -0.05721(14) 0.0176(6) Uani 1 1 d . . . C14 C 0.4951(2) 0.2713(2) -0.04549(15) 0.0216(7) Uani 1 1 d . . . H14 H 0.4737 0.2191 -0.0364 0.026 Uiso 1 1 calc R . . C15 C 0.5857(2) 0.2812(2) -0.04710(17) 0.0306(8) Uani 1 1 d . . . H15 H 0.6272 0.2361 -0.0383 0.037 Uiso 1 1 calc R . . C16 C 0.6187(3) 0.3575(2) -0.06164(19) 0.0342(9) Uani 1 1 d . . . H16 H 0.6821 0.3636 -0.0630 0.041 Uiso 1 1 calc R . . C17 C 0.5602(2) 0.4222(2) -0.07372(17) 0.0297(8) Uani 1 1 d . . . H17 H 0.5830 0.4733 -0.0840 0.036 Uiso 1 1 calc R . . C18 C 0.4656(2) 0.4153(2) -0.07132(15) 0.0219(7) Uani 1 1 d . . . C19 C 0.4051(2) 0.4829(2) -0.08061(15) 0.0232(7) Uani 1 1 d . . . H19 H 0.4271 0.5344 -0.0905 0.028 Uiso 1 1 calc R . . C20 C 0.3154(2) 0.47551(19) -0.07558(14) 0.0190(6) Uani 1 1 d . . . H20 H 0.2755 0.5217 -0.0817 0.023 Uiso 1 1 calc R . . C21 C 0.06945(19) 0.44734(18) 0.05159(13) 0.0136(6) Uani 1 1 d . . . C22 C 0.00653(19) 0.43604(17) 0.08742(13) 0.0117(5) Uani 1 1 d . . . C23 C 0.00672(19) 0.49156(17) 0.13777(13) 0.0132(6) Uani 1 1 d . . . C24 C -0.0614(2) 0.49168(17) 0.17301(14) 0.0146(6) Uani 1 1 d . . . H24 H -0.1100 0.4523 0.1640 0.017 Uiso 1 1 calc R . . C25 C -0.0589(2) 0.54737(19) 0.21984(14) 0.0185(6) Uani 1 1 d . . . H25 H -0.1066 0.5473 0.2419 0.022 Uiso 1 1 calc R . . C26 C 0.0141(2) 0.60481(19) 0.23557(14) 0.0188(6) Uani 1 1 d . . . H26 H 0.0169 0.6420 0.2691 0.023 Uiso 1 1 calc R . . C27 C 0.0804(2) 0.60652(18) 0.20239(14) 0.0173(6) Uani 1 1 d . . . H27 H 0.1295 0.6452 0.2132 0.021 Uiso 1 1 calc R . . C28 C 0.0781(2) 0.55232(18) 0.15218(13) 0.0143(6) Uani 1 1 d . . . C29 C 0.1431(2) 0.55868(18) 0.11464(14) 0.0166(6) Uani 1 1 d . . . H29 H 0.1912 0.5984 0.1247 0.020 Uiso 1 1 calc R . . C30 C 0.1378(2) 0.50897(18) 0.06450(13) 0.0149(6) Uani 1 1 d . . . H30 H 0.1798 0.5157 0.0384 0.018 Uiso 1 1 calc R . . C31 C -0.0716(2) 0.30413(17) 0.13798(13) 0.0131(6) Uani 1 1 d . . . C32 C 0.0112(2) 0.28397(17) 0.17925(14) 0.0149(6) Uani 1 1 d . . . C33 C 0.0145(2) 0.24840(19) 0.23765(14) 0.0184(6) Uani 1 1 d . . . H33 H 0.0727 0.2397 0.2666 0.022 Uiso 1 1 calc R . . C34 C -0.0660(2) 0.22645(19) 0.25261(15) 0.0205(7) Uani 1 1 d . . . H34 H -0.0635 0.2023 0.2922 0.025 Uiso 1 1 calc R . . C35 C -0.1532(2) 0.23901(18) 0.21020(14) 0.0172(6) Uani 1 1 d . . . C36 C -0.2377(2) 0.2139(2) 0.22419(16) 0.0236(7) Uani 1 1 d . . . H36 H -0.2358 0.1869 0.2627 0.028 Uiso 1 1 calc R . . C37 C -0.3212(2) 0.2279(2) 0.18353(17) 0.0266(8) Uani 1 1 d . . . H37 H -0.3771 0.2111 0.1938 0.032 Uiso 1 1 calc R . . C38 C -0.3250(2) 0.2671(2) 0.12625(17) 0.0258(7) Uani 1 1 d . . . H38 H -0.3836 0.2756 0.0977 0.031 Uiso 1 1 calc R . . C39 C -0.2457(2) 0.29312(19) 0.11102(15) 0.0192(6) Uani 1 1 d . . . H39 H -0.2499 0.3204 0.0724 0.023 Uiso 1 1 calc R . . C40 C -0.1572(2) 0.27978(17) 0.15236(14) 0.0152(6) Uani 1 1 d . . . C41 C 0.19694(19) 0.09956(17) 0.20180(13) 0.0135(6) Uani 1 1 d . . . C42 C 0.22782(19) 0.05338(18) 0.15898(13) 0.0134(6) Uani 1 1 d . . . C43 C 0.23219(19) -0.03337(18) 0.16602(14) 0.0140(6) Uani 1 1 d . . . C44 C 0.2643(2) -0.0852(2) 0.12443(15) 0.0214(7) Uani 1 1 d . . . H44 H 0.2862 -0.0623 0.0910 0.026 Uiso 1 1 calc R . . C45 C 0.2640(2) -0.1677(2) 0.13193(16) 0.0249(7) Uani 1 1 d . . . H45 H 0.2848 -0.2018 0.1032 0.030 Uiso 1 1 calc R . . C46 C 0.2334(2) -0.20302(19) 0.18140(15) 0.0216(7) Uani 1 1 d . . . H46 H 0.2331 -0.2607 0.1857 0.026 Uiso 1 1 calc R . . C47 C 0.2041(2) -0.15516(18) 0.22336(14) 0.0166(6) Uani 1 1 d . . . H47 H 0.1843 -0.1796 0.2571 0.020 Uiso 1 1 calc R . . C48 C 0.20294(19) -0.06901(18) 0.21717(13) 0.0146(6) Uani 1 1 d . . . C49 C 0.1716(2) -0.01793(19) 0.25982(14) 0.0172(6) Uani 1 1 d . . . H49 H 0.1524 -0.0417 0.2940 0.021 Uiso 1 1 calc R . . C50 C 0.1685(2) 0.06457(18) 0.25276(13) 0.0161(6) Uani 1 1 d . . . H50 H 0.1474 0.0981 0.2817 0.019 Uiso 1 1 calc R . . C51 C 0.0767(2) 0.13550(17) 0.04429(13) 0.0135(6) Uani 1 1 d . . . C52 C 0.15398(19) 0.09463(17) 0.03660(13) 0.0134(6) Uani 1 1 d . . . C53 C 0.1478(2) 0.04638(17) -0.01870(14) 0.0161(6) Uani 1 1 d . . . C54 C 0.2236(2) 0.00196(19) -0.03073(15) 0.0222(7) Uani 1 1 d . . . H54 H 0.2832 0.0056 -0.0025 0.027 Uiso 1 1 calc R . . C55 C 0.2114(3) -0.0464(2) -0.08307(16) 0.0278(8) Uani 1 1 d . . . H55 H 0.2627 -0.0766 -0.0901 0.033 Uiso 1 1 calc R . . C56 C 0.1248(3) -0.0520(2) -0.12632(16) 0.0291(8) Uani 1 1 d . . . H56 H 0.1173 -0.0863 -0.1620 0.035 Uiso 1 1 calc R . . C57 C 0.0513(3) -0.0080(2) -0.11681(15) 0.0250(7) Uani 1 1 d . . . H57 H -0.0069 -0.0108 -0.1468 0.030 Uiso 1 1 calc R . . C58 C 0.0599(2) 0.04173(18) -0.06323(14) 0.0176(6) Uani 1 1 d . . . C59 C -0.0168(2) 0.08575(19) -0.05264(14) 0.0188(6) Uani 1 1 d . . . H59 H -0.0749 0.0834 -0.0828 0.023 Uiso 1 1 calc R . . C60 C -0.0093(2) 0.13148(18) -0.00014(14) 0.0158(6) Uani 1 1 d . . . H60 H -0.0617 0.1605 0.0065 0.019 Uiso 1 1 calc R . . C61 C 0.5185(3) 0.0806(3) 0.0918(2) 0.0586(14) Uani 1 1 d . . . H61A H 0.5710 0.0780 0.1289 0.088 Uiso 1 1 calc R . . H61B H 0.4680 0.1128 0.1015 0.088 Uiso 1 1 calc R . . H61C H 0.5390 0.1063 0.0572 0.088 Uiso 1 1 calc R . . C62 C 0.4854(3) -0.0015(3) 0.0737(2) 0.0449(11) Uani 1 1 d . . . N N 0.4577(3) -0.0648(2) 0.0571(2) 0.0582(11) 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 I 0.01192(9) 0.02789(12) 0.01807(10) -0.00492(8) 0.00448(7) -0.00370(8) Cu 0.01012(16) 0.01415(18) 0.01475(18) 0.00103(13) 0.00326(14) 0.00016(13) S1 0.0118(3) 0.0156(3) 0.0138(3) 0.0006(3) 0.0048(3) 0.0002(3) S2 0.0135(3) 0.0151(4) 0.0154(3) 0.0003(3) 0.0033(3) -0.0019(3) S3 0.0111(3) 0.0165(4) 0.0156(3) 0.0036(3) 0.0036(3) -0.0009(3) P1 0.0107(3) 0.0141(4) 0.0126(3) 0.0012(3) 0.0047(3) 0.0013(3) P2 0.0106(3) 0.0122(4) 0.0138(3) 0.0012(3) 0.0018(3) -0.0008(3) O1 0.0122(9) 0.0165(11) 0.0159(10) -0.0021(8) 0.0063(8) -0.0019(8) O2 0.0135(10) 0.0174(11) 0.0172(10) 0.0042(8) 0.0077(8) 0.0018(8) O3 0.0116(9) 0.0180(11) 0.0139(10) -0.0015(8) 0.0042(8) 0.0035(8) O4 0.0111(9) 0.0141(10) 0.0176(10) 0.0011(8) 0.0048(8) -0.0012(8) O5 0.0179(10) 0.0107(10) 0.0135(10) 0.0008(8) 0.0007(8) -0.0005(8) O6 0.0102(9) 0.0168(10) 0.0140(10) -0.0026(8) 0.0032(8) -0.0019(8) C1 0.0161(14) 0.0119(14) 0.0143(14) 0.0014(11) 0.0061(11) 0.0015(11) C2 0.0151(14) 0.0146(14) 0.0133(14) 0.0006(11) 0.0049(11) -0.0020(11) C3 0.0185(14) 0.0132(14) 0.0153(14) 0.0024(11) 0.0076(12) 0.0004(11) C4 0.0173(15) 0.0207(16) 0.0197(16) -0.0013(12) 0.0054(12) -0.0001(12) C5 0.0214(16) 0.0251(17) 0.0265(17) -0.0020(14) 0.0138(14) 0.0039(13) C6 0.0293(17) 0.0185(16) 0.0227(16) -0.0037(13) 0.0109(14) 0.0011(14) C7 0.0253(16) 0.0206(16) 0.0172(15) -0.0011(12) 0.0032(13) -0.0005(13) C8 0.0205(15) 0.0156(15) 0.0150(14) 0.0032(11) 0.0054(12) -0.0002(12) C9 0.0193(14) 0.0168(15) 0.0132(14) 0.0015(11) -0.0004(12) 0.0000(12) C10 0.0143(14) 0.0160(15) 0.0178(15) 0.0025(11) 0.0034(12) 0.0014(11) C11 0.0152(14) 0.0203(15) 0.0115(14) -0.0016(11) 0.0063(11) -0.0023(12) C12 0.0146(13) 0.0160(14) 0.0131(13) -0.0009(11) 0.0060(11) -0.0041(11) C13 0.0175(14) 0.0224(16) 0.0142(14) -0.0045(12) 0.0066(12) -0.0033(12) C14 0.0171(15) 0.0274(17) 0.0233(16) -0.0039(13) 0.0107(13) -0.0018(13) C15 0.0185(16) 0.040(2) 0.037(2) -0.0041(16) 0.0150(15) 0.0008(15) C16 0.0209(17) 0.044(2) 0.045(2) -0.0075(18) 0.0211(17) -0.0074(16) C17 0.0255(18) 0.034(2) 0.034(2) -0.0035(16) 0.0165(16) -0.0133(15) C18 0.0198(15) 0.0287(18) 0.0202(16) -0.0049(13) 0.0110(13) -0.0053(13) C19 0.0286(17) 0.0211(17) 0.0221(17) -0.0006(13) 0.0104(14) -0.0115(14) C20 0.0246(16) 0.0156(15) 0.0170(15) -0.0007(12) 0.0056(13) -0.0011(12) C21 0.0126(13) 0.0151(14) 0.0124(13) 0.0010(11) 0.0017(11) 0.0048(11) C22 0.0104(12) 0.0108(13) 0.0133(13) 0.0023(10) 0.0014(11) 0.0012(10) C23 0.0118(13) 0.0143(14) 0.0137(14) 0.0027(11) 0.0037(11) 0.0033(11) C24 0.0140(14) 0.0115(14) 0.0198(15) 0.0004(11) 0.0071(12) 0.0001(11) C25 0.0206(15) 0.0183(16) 0.0191(15) 0.0037(12) 0.0100(13) 0.0012(12) C26 0.0239(16) 0.0166(15) 0.0163(15) -0.0019(12) 0.0058(13) 0.0008(12) C27 0.0175(14) 0.0153(15) 0.0183(15) -0.0010(12) 0.0030(12) 0.0006(12) C28 0.0129(13) 0.0160(15) 0.0136(14) 0.0021(11) 0.0027(11) 0.0021(11) C29 0.0115(13) 0.0173(15) 0.0206(15) 0.0008(12) 0.0030(12) -0.0036(11) C30 0.0121(13) 0.0200(15) 0.0143(14) 0.0059(11) 0.0064(11) 0.0020(11) C31 0.0143(13) 0.0112(14) 0.0152(14) -0.0002(10) 0.0060(11) 0.0000(11) C32 0.0151(14) 0.0117(14) 0.0194(15) -0.0028(11) 0.0073(12) -0.0011(11) C33 0.0207(15) 0.0175(15) 0.0168(15) 0.0007(12) 0.0042(12) 0.0034(12) C34 0.0277(17) 0.0206(16) 0.0163(15) 0.0011(12) 0.0113(13) 0.0024(13) C35 0.0207(15) 0.0103(14) 0.0240(16) -0.0029(12) 0.0123(13) 0.0002(12) C36 0.0288(18) 0.0182(16) 0.0309(18) -0.0018(13) 0.0211(15) -0.0028(13) C37 0.0195(16) 0.0277(18) 0.038(2) -0.0065(15) 0.0183(15) -0.0071(14) C38 0.0159(15) 0.0242(18) 0.039(2) -0.0058(15) 0.0097(15) -0.0030(13) C39 0.0163(15) 0.0186(16) 0.0232(16) -0.0034(12) 0.0057(13) 0.0003(12) C40 0.0146(14) 0.0121(14) 0.0207(15) -0.0045(11) 0.0079(12) -0.0012(11) C41 0.0119(13) 0.0124(14) 0.0138(14) 0.0005(11) -0.0011(11) -0.0022(11) C42 0.0095(12) 0.0164(15) 0.0136(14) 0.0033(11) 0.0013(11) -0.0008(11) C43 0.0086(12) 0.0151(14) 0.0183(15) 0.0027(11) 0.0031(11) 0.0036(11) C44 0.0226(16) 0.0219(17) 0.0231(16) 0.0045(13) 0.0122(13) 0.0064(13) C45 0.0303(18) 0.0191(16) 0.0293(18) 0.0029(13) 0.0152(15) 0.0093(14) C46 0.0238(16) 0.0130(15) 0.0280(17) 0.0044(13) 0.0065(14) 0.0039(13) C47 0.0153(14) 0.0168(15) 0.0175(15) 0.0055(11) 0.0037(12) 0.0007(11) C48 0.0102(13) 0.0159(15) 0.0157(14) 0.0034(11) -0.0005(11) -0.0015(11) C49 0.0195(15) 0.0191(16) 0.0129(14) 0.0041(11) 0.0039(12) -0.0023(12) C50 0.0172(14) 0.0179(15) 0.0120(14) -0.0006(11) 0.0013(11) -0.0002(12) C51 0.0144(14) 0.0133(14) 0.0129(14) 0.0020(11) 0.0038(11) -0.0033(11) C52 0.0124(13) 0.0134(14) 0.0144(14) 0.0042(11) 0.0034(11) -0.0017(11) C53 0.0218(15) 0.0113(14) 0.0169(15) 0.0019(11) 0.0082(12) -0.0035(12) C54 0.0278(17) 0.0195(16) 0.0213(16) 0.0027(13) 0.0101(14) 0.0033(13) C55 0.039(2) 0.0232(18) 0.0265(18) 0.0012(14) 0.0177(16) 0.0072(15) C56 0.051(2) 0.0171(17) 0.0207(17) -0.0030(13) 0.0117(16) -0.0010(16) C57 0.0373(19) 0.0196(17) 0.0171(16) -0.0006(13) 0.0048(14) -0.0070(14) C58 0.0260(16) 0.0122(14) 0.0152(14) 0.0026(11) 0.0064(13) -0.0054(12) C59 0.0185(15) 0.0207(16) 0.0154(15) 0.0019(12) 0.0006(12) -0.0079(12) C60 0.0110(13) 0.0193(15) 0.0176(15) 0.0026(12) 0.0044(12) -0.0028(11) C61 0.042(2) 0.074(4) 0.066(3) -0.041(3) 0.024(2) -0.025(2) C62 0.030(2) 0.053(3) 0.052(3) 0.004(2) 0.012(2) 0.006(2) N 0.042(2) 0.040(2) 0.096(3) 0.012(2) 0.023(2) 0.0046(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I Cu 2.4925(4) . ? Cu P2 2.2077(8) . ? Cu P1 2.2123(8) . ? S1 C2 1.773(3) . ? S1 C12 1.788(3) . ? S2 C31 1.781(3) . ? S2 C22 1.783(3) . ? S3 C42 1.775(3) . ? S3 C52 1.781(3) . ? P1 O1 1.609(2) . ? P1 O3 1.615(2) . ? P1 O2 1.624(2) . ? P2 O4 1.606(2) . ? P2 O6 1.617(2) . ? P2 O5 1.627(2) . ? O1 C1 1.379(3) . ? O2 C11 1.389(3) . ? O3 C21 1.395(3) . ? O4 C32 1.398(3) . ? O5 C41 1.390(3) . ? O6 C51 1.391(3) . ? C1 C2 1.372(4) . ? C1 C10 1.403(4) . ? C2 C3 1.438(4) . ? C3 C8 1.418(4) . ? C3 C4 1.422(4) . ? C4 C5 1.364(4) . ? C4 H4 0.9500 . ? C5 C6 1.406(5) . ? C5 H5 0.9500 . ? C6 C7 1.357(5) . ? C6 H6 0.9500 . ? C7 C8 1.422(4) . ? C7 H7 0.9500 . ? C8 C9 1.411(4) . ? C9 C10 1.364(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.369(4) . ? C11 C20 1.403(4) . ? C12 C13 1.438(4) . ? C13 C14 1.415(4) . ? C13 C18 1.425(4) . ? C14 C15 1.359(4) . ? C14 H14 0.9500 . ? C15 C16 1.408(5) . ? C15 H15 0.9500 . ? C16 C17 1.355(5) . ? C16 H16 0.9500 . ? C17 C18 1.419(4) . ? C17 H17 0.9500 . ? C18 C19 1.408(5) . ? C19 C20 1.364(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.371(4) . ? C21 C30 1.409(4) . ? C22 C23 1.433(4) . ? C23 C24 1.413(4) . ? C23 C28 1.430(4) . ? C24 C25 1.370(4) . ? C24 H24 0.9500 . ? C25 C26 1.411(4) . ? C25 H25 0.9500 . ? C26 C27 1.357(4) . ? C26 H26 0.9500 . ? C27 C28 1.412(4) . ? C27 H27 0.9500 . ? C28 C29 1.416(4) . ? C29 C30 1.358(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.376(4) . ? C31 C40 1.435(4) . ? C32 C33 1.401(4) . ? C33 C34 1.359(4) . ? C33 H33 0.9500 . ? C34 C35 1.412(4) . ? C34 H34 0.9500 . ? C35 C36 1.419(4) . ? C35 C40 1.426(4) . ? C36 C37 1.357(5) . ? C36 H36 0.9500 . ? C37 C38 1.404(5) . ? C37 H37 0.9500 . ? C38 C39 1.365(4) . ? C38 H38 0.9500 . ? C39 C40 1.419(4) . ? C39 H39 0.9500 . ? C41 C42 1.371(4) . ? C41 C50 1.412(4) . ? C42 C43 1.430(4) . ? C43 C44 1.412(4) . ? C43 C48 1.426(4) . ? C44 C45 1.364(4) . ? C44 H44 0.9500 . ? C45 C46 1.401(5) . ? C45 H45 0.9500 . ? C46 C47 1.360(4) . ? C46 H46 0.9500 . ? C47 C48 1.419(4) . ? C47 H47 0.9500 . ? C48 C49 1.417(4) . ? C49 C50 1.361(4) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.371(4) . ? C51 C60 1.406(4) . ? C52 C53 1.435(4) . ? C53 C54 1.414(4) . ? C53 C58 1.429(4) . ? C54 C55 1.373(5) . ? C54 H54 0.9500 . ? C55 C56 1.401(5) . ? C55 H55 0.9500 . ? C56 C57 1.363(5) . ? C56 H56 0.9500 . ? C57 C58 1.414(4) . ? C57 H57 0.9500 . ? C58 C59 1.411(5) . ? C59 C60 1.359(4) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.455(7) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 N 1.144(6) . ? 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 P2 Cu P1 108.62(3) . . ? P2 Cu I 123.79(2) . . ? P1 Cu I 127.57(2) . . ? C2 S1 C12 102.99(13) . . ? C31 S2 C22 103.86(13) . . ? C42 S3 C52 100.46(13) . . ? O1 P1 O3 93.43(11) . . ? O1 P1 O2 100.73(11) . . ? O3 P1 O2 99.81(11) . . ? O1 P1 Cu 118.75(8) . . ? O3 P1 Cu 115.69(8) . . ? O2 P1 Cu 123.02(8) . . ? O4 P2 O6 100.10(10) . . ? O4 P2 O5 99.54(11) . . ? O6 P2 O5 99.91(11) . . ? O4 P2 Cu 109.40(8) . . ? O6 P2 Cu 117.83(8) . . ? O5 P2 Cu 125.91(8) . . ? C1 O1 P1 127.30(18) . . ? C11 O2 P1 123.83(18) . . ? C21 O3 P1 118.91(17) . . ? C32 O4 P2 123.86(18) . . ? C41 O5 P2 125.21(18) . . ? C51 O6 P2 126.49(18) . . ? C2 C1 O1 123.4(3) . . ? C2 C1 C10 121.7(3) . . ? O1 C1 C10 114.8(3) . . ? C1 C2 C3 119.5(3) . . ? C1 C2 S1 119.3(2) . . ? C3 C2 S1 120.8(2) . . ? C8 C3 C4 118.8(3) . . ? C8 C3 C2 118.3(3) . . ? C4 C3 C2 122.9(3) . . ? C5 C4 C3 120.3(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.1(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 119.8(3) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 121.2(3) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C3 119.7(3) . . ? C9 C8 C7 121.6(3) . . ? C3 C8 C7 118.7(3) . . ? C10 C9 C8 121.1(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C1 119.6(3) . . ? C9 C10 H10 120.2 . . ? C1 C10 H10 120.2 . . ? C12 C11 O2 123.0(3) . . ? C12 C11 C20 121.8(3) . . ? O2 C11 C20 115.2(3) . . ? C11 C12 C13 119.3(3) . . ? C11 C12 S1 120.6(2) . . ? C13 C12 S1 119.9(2) . . ? C14 C13 C18 118.7(3) . . ? C14 C13 C12 122.8(3) . . ? C18 C13 C12 118.4(3) . . ? C15 C14 C13 120.8(3) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.7(3) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 121.3(3) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 122.0(3) . . ? C19 C18 C13 119.5(3) . . ? C17 C18 C13 118.4(3) . . ? C20 C19 C18 121.0(3) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C11 119.8(3) . . ? C19 C20 H20 120.1 . . ? C11 C20 H20 120.1 . . ? C22 C21 O3 119.3(3) . . ? C22 C21 C30 122.4(3) . . ? O3 C21 C30 118.2(3) . . ? C21 C22 C23 119.0(3) . . ? C21 C22 S2 117.7(2) . . ? C23 C22 S2 123.2(2) . . ? C24 C23 C28 117.7(3) . . ? C24 C23 C22 123.9(3) . . ? C28 C23 C22 118.5(3) . . ? C25 C24 C23 121.4(3) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 120.6(3) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 119.4(3) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 121.6(3) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C27 C28 C29 121.3(3) . . ? C27 C28 C23 119.2(3) . . ? C29 C28 C23 119.5(3) . . ? C30 C29 C28 121.1(3) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C21 119.4(3) . . ? C29 C30 H30 120.3 . . ? C21 C30 H30 120.3 . . ? C32 C31 C40 118.6(3) . . ? C32 C31 S2 122.3(2) . . ? C40 C31 S2 119.0(2) . . ? C31 C32 O4 118.6(3) . . ? C31 C32 C33 122.2(3) . . ? O4 C32 C33 119.2(3) . . ? C34 C33 C32 119.7(3) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 121.0(3) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C36 121.8(3) . . ? C34 C35 C40 119.4(3) . . ? C36 C35 C40 118.8(3) . . ? C37 C36 C35 121.1(3) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 120.1(3) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 120.9(3) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C38 C39 C40 120.6(3) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C35 118.4(3) . . ? C39 C40 C31 122.9(3) . . ? C35 C40 C31 118.7(3) . . ? C42 C41 O5 122.3(3) . . ? C42 C41 C50 122.3(3) . . ? O5 C41 C50 115.3(3) . . ? C41 C42 C43 119.2(3) . . ? C41 C42 S3 119.1(2) . . ? C43 C42 S3 121.7(2) . . ? C44 C43 C48 118.6(3) . . ? C44 C43 C42 122.8(3) . . ? C48 C43 C42 118.6(3) . . ? C45 C44 C43 120.5(3) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 121.0(3) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C47 C46 C45 120.4(3) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 120.5(3) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C49 C48 C47 121.5(3) . . ? C49 C48 C43 119.4(3) . . ? C47 C48 C43 119.0(3) . . ? C50 C49 C48 121.3(3) . . ? C50 C49 H49 119.4 . . ? C48 C49 H49 119.4 . . ? C49 C50 C41 119.1(3) . . ? C49 C50 H50 120.5 . . ? C41 C50 H50 120.5 . . ? C52 C51 O6 122.6(3) . . ? C52 C51 C60 122.2(3) . . ? O6 C51 C60 115.1(3) . . ? C51 C52 C53 119.4(3) . . ? C51 C52 S3 119.1(2) . . ? C53 C52 S3 121.5(2) . . ? C54 C53 C58 118.4(3) . . ? C54 C53 C52 123.5(3) . . ? C58 C53 C52 118.0(3) . . ? C55 C54 C53 120.4(3) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 121.3(3) . . ? C54 C55 H55 119.3 . . ? C56 C55 H55 119.3 . . ? C57 C56 C55 119.5(3) . . ? C57 C56 H56 120.2 . . ? C55 C56 H56 120.2 . . ? C56 C57 C58 121.3(3) . . ? C56 C57 H57 119.3 . . ? C58 C57 H57 119.3 . . ? C59 C58 C57 121.3(3) . . ? C59 C58 C53 119.7(3) . . ? C57 C58 C53 119.0(3) . . ? C60 C59 C58 121.3(3) . . ? C60 C59 H59 119.4 . . ? C58 C59 H59 119.4 . . ? C59 C60 C51 119.4(3) . . ? C59 C60 H60 120.3 . . ? C51 C60 H60 120.3 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N C62 C61 177.2(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.958 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.107 # Attachment 'msb351_0m.cif' data_msb351_0m _database_code_depnum_ccdc_archive 'CCDC 672313' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H44 Cu I2.33 N2 O6 P2 S3' _chemical_formula_sum 'C70 H44 Cu I2.33 N2 O6 P2 S3' _chemical_formula_weight 1526.83 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnn2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 38.803(3) _cell_length_b 13.801(1) _cell_length_c 17.579(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9414(1) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 23.81 _exptl_crystal_description Block _exptl_crystal_colour Yellow-orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4540 _exptl_absorpt_coefficient_mu 1.702 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7126 _exptl_absorpt_correction_T_max 0.8244 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; The data were collected using three sets of 606 frames, each frame having an 0.3 deg width in omega, at phi = 0, 120 and 240 deg. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59913 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 23.82 _reflns_number_total 14459 _reflns_number_gt 12332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2006)' _publ_section_references ; Bruker-AXS (2006). APEX2, Version 2.1-0, Madison, WI. Bruker-AXS (2006a). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2007). SADABS, Version 2007/2. University of G\"ottingen, Germany. Sheldrick, G, M. (2005). CELL_NOW. University of G\"ottingen, Germany. Spek, A. L. (2007). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 \%A) and included as riding contributions with isotropic displacement parameters 1.2 times those of the attached carbon atoms. The bipyridyl ligand attached to Cu2 is not symmetrically disposed with respect to the 2-fold axis passing through this cation and consequently is disordered over two equally populated sites. This ligand was refined subject to being restrained to have approximately the same geometry as that in the ordered cation. Two isolated residual density peaks of height ca. 7 electrons/\%A^3^ which could not be identified as part of any reasonable component of the structure were removed using the SQUEEZE option of PLATON (Spek, 2007). The crystal proved to be a racemic twin and was refined accordingly. ; _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^)+(0.0463P)^2^+40.6056P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.254(18) _refine_ls_number_reflns 14459 _refine_ls_number_parameters 1219 _refine_ls_number_restraints 112 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 I1 I 0.822885(19) 0.43221(6) 0.43420(5) 0.0613(2) Uani 1 1 d . . . I2 I 0.821651(16) 0.55768(6) 0.56214(5) 0.05017(19) Uani 1 1 d . . . I3 I 0.82078(2) 0.68039(9) 0.69332(6) 0.0827(3) Uani 1 1 d . . . I4 I 0.0000 0.0000 0.14776(6) 0.0465(3) Uani 1 2 d S . . Cu1 Cu 0.82131(2) 0.57071(7) 0.06305(6) 0.0215(2) Uani 1 1 d . . . S1 S 0.78814(6) 0.30223(15) 0.04413(12) 0.0231(5) Uani 1 1 d . . . S2 S 0.95050(5) 0.56537(17) 0.05226(13) 0.0255(5) Uani 1 1 d . . . S3 S 0.79100(6) 0.83437(16) 0.08397(12) 0.0221(5) Uani 1 1 d . . . P1 P 0.84991(5) 0.45021(16) 0.00821(12) 0.0188(5) Uani 1 1 d . . . P2 P 0.85343(6) 0.68717(16) 0.11408(13) 0.0207(5) Uani 1 1 d . . . O1 O 0.86138(14) 0.3544(4) 0.0516(3) 0.0253(14) Uani 1 1 d . . . O2 O 0.83463(13) 0.4068(4) -0.0704(3) 0.0175(12) Uani 1 1 d . . . O3 O 0.88783(14) 0.4806(4) -0.0232(3) 0.0246(14) Uani 1 1 d . . . O4 O 0.89171(13) 0.6563(4) 0.1388(3) 0.0212(13) Uani 1 1 d . . . O5 O 0.86449(14) 0.7828(4) 0.0680(3) 0.0245(13) Uani 1 1 d . . . O6 O 0.84047(14) 0.7313(4) 0.1946(3) 0.0217(13) Uani 1 1 d . . . N1 N 0.78086(18) 0.5237(5) 0.1295(4) 0.0257(18) Uani 1 1 d . . . N2 N 0.78135(17) 0.6190(5) -0.0027(4) 0.0209(16) Uani 1 1 d . . . C1 C 0.8558(2) 0.2612(7) 0.0237(5) 0.026(2) Uani 1 1 d . . . C2 C 0.8842(2) 0.2051(6) 0.0049(5) 0.023(2) Uani 1 1 d . . . H2 H 0.9068 0.2287 0.0150 0.027 Uiso 1 1 calc R . . C3 C 0.8800(2) 0.1167(7) -0.0279(5) 0.029(2) Uani 1 1 d . . . H3 H 0.8997 0.0796 -0.0418 0.035 Uiso 1 1 calc R . . C4 C 0.8464(2) 0.0794(6) -0.0414(5) 0.024(2) Uani 1 1 d . . . C5 C 0.8418(2) -0.0135(6) -0.0739(5) 0.027(2) Uani 1 1 d . . . H5 H 0.8614 -0.0506 -0.0882 0.032 Uiso 1 1 calc R . . C6 C 0.8097(3) -0.0502(6) -0.0848(5) 0.033(2) Uani 1 1 d . . . H6 H 0.8068 -0.1109 -0.1095 0.040 Uiso 1 1 calc R . . C7 C 0.7806(2) 0.0024(7) -0.0592(5) 0.029(2) Uani 1 1 d . . . H7 H 0.7583 -0.0252 -0.0647 0.035 Uiso 1 1 calc R . . C8 C 0.7840(2) 0.0921(6) -0.0267(5) 0.025(2) Uani 1 1 d . . . H8 H 0.7641 0.1263 -0.0098 0.030 Uiso 1 1 calc R . . C9 C 0.8179(2) 0.1346(6) -0.0184(5) 0.025(2) Uani 1 1 d . . . C10 C 0.8220(2) 0.2279(6) 0.0137(5) 0.0190(18) Uani 1 1 d . . . C11 C 0.7759(2) 0.3612(6) -0.0410(5) 0.0198(19) Uani 1 1 d . . . C12 C 0.7402(2) 0.3692(6) -0.0596(5) 0.027(2) Uani 1 1 d . . . C13 C 0.7130(2) 0.3320(7) -0.0127(5) 0.027(2) Uani 1 1 d . . . H13 H 0.7187 0.2962 0.0317 0.033 Uiso 1 1 calc R . . C14 C 0.6793(2) 0.3465(7) -0.0301(6) 0.033(2) Uani 1 1 d . . . H14 H 0.6618 0.3209 0.0019 0.040 Uiso 1 1 calc R . . C15 C 0.6704(2) 0.3992(7) -0.0952(6) 0.038(3) Uani 1 1 d . . . H15 H 0.6467 0.4109 -0.1056 0.046 Uiso 1 1 calc R . . C16 C 0.6948(2) 0.4344(7) -0.1447(6) 0.040(3) Uani 1 1 d . . . H16 H 0.6880 0.4666 -0.1900 0.048 Uiso 1 1 calc R . . C17 C 0.7305(2) 0.4223(7) -0.1275(6) 0.031(2) Uani 1 1 d . . . C18 C 0.7565(2) 0.4574(6) -0.1746(5) 0.026(2) Uani 1 1 d . . . H18 H 0.7504 0.4881 -0.2211 0.031 Uiso 1 1 calc R . . C19 C 0.7901(2) 0.4492(6) -0.1564(5) 0.0206(19) Uani 1 1 d . . . H19 H 0.8072 0.4732 -0.1902 0.025 Uiso 1 1 calc R . . C20 C 0.80001(18) 0.4048(6) -0.0871(4) 0.0158(18) Uani 1 1 d . . . C21 C 0.8944(2) 0.5748(6) -0.0461(5) 0.021(2) Uani 1 1 d . . . C22 C 0.8747(2) 0.6177(7) -0.1025(5) 0.028(2) Uani 1 1 d . . . H22 H 0.8556 0.5839 -0.1233 0.034 Uiso 1 1 calc R . . C23 C 0.8825(2) 0.7081(7) -0.1283(6) 0.037(2) Uani 1 1 d . . . H23 H 0.8687 0.7364 -0.1670 0.044 Uiso 1 1 calc R . . C24 C 0.9111(2) 0.7614(7) -0.0984(6) 0.035(2) Uani 1 1 d . . . C25 C 0.9210(3) 0.8516(7) -0.1251(7) 0.041(3) Uani 1 1 d . . . H25 H 0.9091 0.8789 -0.1672 0.050 Uiso 1 1 calc R . . C26 C 0.9474(3) 0.9024(7) -0.0928(7) 0.045(3) Uani 1 1 d . . . H26 H 0.9535 0.9639 -0.1131 0.054 Uiso 1 1 calc R . . C27 C 0.9658(3) 0.8662(7) -0.0306(6) 0.040(3) Uani 1 1 d . . . H27 H 0.9835 0.9029 -0.0068 0.048 Uiso 1 1 calc R . . C28 C 0.9571(2) 0.7749(7) -0.0053(6) 0.037(3) Uani 1 1 d . . . H28 H 0.9698 0.7484 0.0361 0.045 Uiso 1 1 calc R . . C29 C 0.9302(2) 0.7181(6) -0.0379(5) 0.0204(19) Uani 1 1 d . . . C30 C 0.9216(2) 0.6229(6) -0.0129(5) 0.022(2) Uani 1 1 d . . . C31 C 0.9237(2) 0.5104(6) 0.1223(4) 0.0179(18) Uani 1 1 d . . . C32 C 0.9322(2) 0.4128(6) 0.1446(5) 0.0221(19) Uani 1 1 d . . . C33 C 0.9563(2) 0.3540(6) 0.1060(5) 0.023(2) Uani 1 1 d . . . H33 H 0.9677 0.3782 0.0622 0.027 Uiso 1 1 calc R . . C34 C 0.9632(2) 0.2624(7) 0.1316(5) 0.030(2) Uani 1 1 d . . . H34 H 0.9784 0.2216 0.1038 0.035 Uiso 1 1 calc R . . C35 C 0.9478(2) 0.2285(7) 0.1995(5) 0.028(2) Uani 1 1 d . . . H35 H 0.9539 0.1664 0.2184 0.034 Uiso 1 1 calc R . . C36 C 0.9251(2) 0.2812(7) 0.2371(5) 0.030(2) Uani 1 1 d . . . H36 H 0.9157 0.2571 0.2832 0.036 Uiso 1 1 calc R . . C37 C 0.9146(2) 0.3739(7) 0.2096(5) 0.026(2) Uani 1 1 d . . . C38 C 0.8886(2) 0.4299(7) 0.2475(5) 0.024(2) Uani 1 1 d . . . H38 H 0.8773 0.4050 0.2913 0.029 Uiso 1 1 calc R . . C39 C 0.8805(2) 0.5184(7) 0.2204(5) 0.025(2) Uani 1 1 d . . . H39 H 0.8621 0.5538 0.2431 0.030 Uiso 1 1 calc R . . C40 C 0.8985(2) 0.5587(6) 0.1596(5) 0.022(2) Uani 1 1 d . . . C41 C 0.8594(2) 0.8758(6) 0.0991(5) 0.022(2) Uani 1 1 d . . . C42 C 0.8891(2) 0.9319(6) 0.1141(5) 0.023(2) Uani 1 1 d . . . H42 H 0.9115 0.9083 0.1024 0.028 Uiso 1 1 calc R . . C43 C 0.8844(2) 1.0213(6) 0.1460(5) 0.028(2) Uani 1 1 d . . . H43 H 0.9041 1.0595 0.1579 0.034 Uiso 1 1 calc R . . C44 C 0.8510(2) 1.0589(6) 0.1619(5) 0.023(2) Uani 1 1 d . . . C45 C 0.8461(2) 1.1505(6) 0.1955(5) 0.029(2) Uani 1 1 d . . . H45 H 0.8658 1.1881 0.2084 0.035 Uiso 1 1 calc R . . C46 C 0.8139(3) 1.1878(7) 0.2105(5) 0.033(2) Uani 1 1 d . . . H46 H 0.8112 1.2482 0.2358 0.040 Uiso 1 1 calc R . . C47 C 0.7850(3) 1.1331(7) 0.1871(5) 0.035(2) Uani 1 1 d . . . H47 H 0.7626 1.1598 0.1924 0.042 Uiso 1 1 calc R . . C48 C 0.7888(2) 1.0437(6) 0.1575(5) 0.0216(19) Uani 1 1 d . . . H48 H 0.7687 1.0069 0.1464 0.026 Uiso 1 1 calc R . . C49 C 0.8209(2) 1.0031(6) 0.1425(5) 0.0225(19) Uani 1 1 d . . . C50 C 0.8265(2) 0.9090(6) 0.1104(4) 0.0172(18) Uani 1 1 d . . . C51 C 0.7807(2) 0.7750(6) 0.1712(5) 0.0192(19) Uani 1 1 d . . . C52 C 0.7446(2) 0.7677(6) 0.1917(5) 0.0172(18) Uani 1 1 d . . . C53 C 0.7182(2) 0.8049(6) 0.1494(6) 0.0236(19) Uani 1 1 d . . . H53 H 0.7233 0.8427 0.1057 0.028 Uiso 1 1 calc R . . C54 C 0.6848(3) 0.7890(7) 0.1685(6) 0.036(2) Uani 1 1 d . . . H54 H 0.6669 0.8104 0.1359 0.043 Uiso 1 1 calc R . . C55 C 0.6768(2) 0.7402(8) 0.2375(6) 0.037(2) Uani 1 1 d . . . H55 H 0.6534 0.7320 0.2526 0.045 Uiso 1 1 calc R . . C56 C 0.7025(2) 0.7056(6) 0.2812(5) 0.027(2) Uani 1 1 d . . . H56 H 0.6970 0.6726 0.3270 0.033 Uiso 1 1 calc R . . C57 C 0.7371(2) 0.7169(6) 0.2608(5) 0.023(2) Uani 1 1 d . . . C58 C 0.7642(2) 0.6795(6) 0.3078(5) 0.026(2) Uani 1 1 d . . . H58 H 0.7588 0.6489 0.3547 0.031 Uiso 1 1 calc R . . C59 C 0.7976(2) 0.6876(6) 0.2855(5) 0.023(2) Uani 1 1 d . . . H59 H 0.8155 0.6646 0.3175 0.027 Uiso 1 1 calc R . . C60 C 0.8054(2) 0.7299(6) 0.2156(5) 0.022(2) Uani 1 1 d . . . C61 C 0.7831(3) 0.4736(7) 0.1939(6) 0.035(2) Uani 1 1 d . . . H61 H 0.8051 0.4616 0.2154 0.042 Uiso 1 1 calc R . . C62 C 0.7540(3) 0.4385(8) 0.2304(6) 0.049(3) Uani 1 1 d . . . H62 H 0.7563 0.4017 0.2758 0.059 Uiso 1 1 calc R . . C63 C 0.7214(3) 0.4573(9) 0.2004(8) 0.059(4) Uani 1 1 d . . . H63 H 0.7010 0.4363 0.2253 0.070 Uiso 1 1 calc R . . C64 C 0.7203(3) 0.5082(8) 0.1323(8) 0.054(3) Uani 1 1 d . . . H64 H 0.6986 0.5203 0.1090 0.065 Uiso 1 1 calc R . . C65 C 0.7502(2) 0.5423(7) 0.0971(6) 0.032(2) Uani 1 1 d . . . C66 C 0.7507(3) 0.5988(7) 0.0269(6) 0.035(2) Uani 1 1 d . . . C67 C 0.7197(3) 0.6277(9) -0.0111(7) 0.051(3) Uani 1 1 d . . . H67 H 0.6976 0.6120 0.0088 0.061 Uiso 1 1 calc R . . C68 C 0.7232(4) 0.6781(10) -0.0761(10) 0.077(5) Uani 1 1 d . . . H68 H 0.7030 0.6979 -0.1022 0.092 Uiso 1 1 calc R . . C69 C 0.7551(4) 0.7026(8) -0.1070(7) 0.052(3) Uani 1 1 d . . . H69 H 0.7575 0.7383 -0.1529 0.063 Uiso 1 1 calc R . . C70 C 0.7829(3) 0.6708(7) -0.0653(7) 0.041(3) Uani 1 1 d . . . H70 H 0.8051 0.6879 -0.0833 0.050 Uiso 1 1 calc R . . Cu2 Cu 1.0000 0.5000 0.53953(8) 0.0318(4) Uani 1 2 d SD . . P3 P 0.97853(6) 0.37542(19) 0.47815(13) 0.0282(6) Uani 1 1 d . . . S4 S 0.99259(6) 0.20960(17) 0.61773(13) 0.0294(5) Uani 1 1 d . . . S5 S 1.0000 0.5000 0.26414(18) 0.0483(11) Uani 1 2 d S . . O7 O 0.94335(14) 0.3289(5) 0.5135(3) 0.0276(15) Uani 1 1 d . . . O8 O 1.00142(16) 0.2800(5) 0.4626(3) 0.0364(17) Uani 1 1 d . . . O9 O 0.96446(14) 0.3916(5) 0.3924(3) 0.0262(14) Uani 1 1 d . . . C71 C 0.9361(2) 0.3314(7) 0.5908(5) 0.032(2) Uani 1 1 d . . . C72 C 0.9074(2) 0.3852(7) 0.6137(5) 0.029(2) Uani 1 1 d . . . H72 H 0.8926 0.4129 0.5765 0.034 Uiso 1 1 calc R . . C73 C 0.9005(2) 0.3980(7) 0.6884(5) 0.032(2) Uani 1 1 d . . . H73 H 0.8815 0.4374 0.7026 0.038 Uiso 1 1 calc R . . C74 C 0.9207(2) 0.3545(6) 0.7462(5) 0.023(2) Uani 1 1 d . . . C75 C 0.9158(2) 0.3723(6) 0.8236(5) 0.031(2) Uani 1 1 d . . . H75 H 0.8970 0.4115 0.8390 0.038 Uiso 1 1 calc R . . C76 C 0.9368(2) 0.3362(7) 0.8772(6) 0.030(2) Uani 1 1 d . . . H76 H 0.9337 0.3531 0.9292 0.037 Uiso 1 1 calc R . . C77 C 0.9639(2) 0.2719(7) 0.8550(5) 0.031(2) Uani 1 1 d . . . H77 H 0.9779 0.2429 0.8929 0.038 Uiso 1 1 calc R . . C78 C 0.9698(2) 0.2517(7) 0.7810(6) 0.036(2) Uani 1 1 d . . . H78 H 0.9879 0.2085 0.7678 0.043 Uiso 1 1 calc R . . C79 C 0.9495(2) 0.2937(6) 0.7229(5) 0.023(2) Uani 1 1 d . . . C80 C 0.9568(2) 0.2809(6) 0.6434(5) 0.026(2) Uani 1 1 d . . . C81 C 0.9794(2) 0.1496(7) 0.5340(5) 0.028(2) Uani 1 1 d . . . C82 C 0.9619(3) 0.0572(7) 0.5359(6) 0.042(3) Uani 1 1 d . . . C83 C 0.9524(3) 0.0131(8) 0.6051(7) 0.043(3) Uani 1 1 d . . . H83 H 0.9577 0.0437 0.6521 0.052 Uiso 1 1 calc R . . C84 C 0.9344(3) -0.0786(8) 0.6049(7) 0.055(3) Uani 1 1 d U . . H84 H 0.9282 -0.1111 0.6504 0.066 Uiso 1 1 calc R . . C85 C 0.9268(3) -0.1172(9) 0.5313(8) 0.060(3) Uani 1 1 d U . . H85 H 0.9142 -0.1761 0.5288 0.072 Uiso 1 1 calc R . . C86 C 0.9358(3) -0.0774(9) 0.4684(8) 0.055(3) Uani 1 1 d U . . H86 H 0.9303 -0.1100 0.4224 0.066 Uiso 1 1 calc R . . C87 C 0.9536(3) 0.0130(9) 0.4634(8) 0.058(4) Uani 1 1 d . . . C88 C 0.9632(3) 0.0583(12) 0.3948(7) 0.066(4) Uani 1 1 d . . . H88 H 0.9581 0.0280 0.3476 0.079 Uiso 1 1 calc R . . C89 C 0.9795(3) 0.1435(10) 0.3956(7) 0.055(3) Uani 1 1 d . . . H89 H 0.9865 0.1731 0.3493 0.066 Uiso 1 1 calc R . . C90 C 0.9863(2) 0.1888(8) 0.4651(6) 0.034(2) Uani 1 1 d . . . C91 C 0.9513(2) 0.4826(7) 0.3768(4) 0.021(2) Uani 1 1 d . . . C92 C 0.9201(2) 0.5103(7) 0.4158(5) 0.026(2) Uani 1 1 d . . . H92 H 0.9098 0.4683 0.4520 0.031 Uiso 1 1 calc R . . C93 C 0.9056(2) 0.5993(7) 0.3995(5) 0.030(2) Uani 1 1 d . . . H93 H 0.8852 0.6184 0.4250 0.036 Uiso 1 1 calc R . . C94 C 0.9204(2) 0.6613(7) 0.3464(5) 0.030(2) Uani 1 1 d . . . C95 C 0.9044(2) 0.7496(7) 0.3288(5) 0.033(2) Uani 1 1 d . . . H95 H 0.8836 0.7677 0.3535 0.039 Uiso 1 1 calc R . . C96 C 0.9191(4) 0.8104(8) 0.2748(7) 0.056(3) Uani 1 1 d . . . H96 H 0.9080 0.8700 0.2631 0.067 Uiso 1 1 calc R . . C97 C 0.9497(3) 0.7864(9) 0.2374(7) 0.052(3) Uani 1 1 d . . . H97 H 0.9599 0.8295 0.2017 0.062 Uiso 1 1 calc R . . C98 C 0.9639(3) 0.7027(9) 0.2530(5) 0.042(3) Uani 1 1 d . . . H98 H 0.9845 0.6864 0.2265 0.050 Uiso 1 1 calc R . . C99 C 0.95082(19) 0.6329(7) 0.3076(5) 0.028(2) Uani 1 1 d . . . C100 C 0.9662(2) 0.5435(8) 0.3240(5) 0.032(2) Uani 1 1 d . . . N3 N 1.0348(3) 0.4280(9) 0.6080(6) 0.028(4) Uani 0.50 1 d PDU . . N4 N 0.9804(3) 0.5297(10) 0.6447(4) 0.039(4) Uani 0.50 1 d PDU . . C101 C 1.0626(3) 0.3751(10) 0.5886(9) 0.023(4) Uani 0.50 1 d PDU . . H10A H 1.0682 0.3683 0.5357 0.028 Uiso 0.50 1 d PR . . C102 C 1.0842(4) 0.3281(12) 0.6398(8) 0.043(5) Uani 0.50 1 d PDU . . H10B H 1.1046 0.2933 0.6252 0.052 Uiso 0.50 1 d PR . . C103 C 1.0752(5) 0.3335(15) 0.7164(9) 0.037(5) Uani 0.50 1 d PDU . . H10C H 1.0883 0.2980 0.7534 0.045 Uiso 0.50 1 d PR . . C104 C 1.0476(5) 0.3910(13) 0.7411(11) 0.024(5) Uani 0.50 1 d PDU . . H10D H 1.0420 0.3981 0.7940 0.029 Uiso 0.50 1 d PR . . C105 C 1.0292(3) 0.4375(11) 0.6827(7) 0.024(4) Uani 0.50 1 d PDU . . C106 C 1.0000 0.5000 0.7026(6) 0.022(3) Uani 1 2 d SDU . . C107 C 0.9895(4) 0.5251(11) 0.7763(8) 0.032(5) Uani 0.50 1 d PDU . . H10E H 1.0025 0.5030 0.8193 0.038 Uiso 0.50 1 d PR . . C108 C 0.9603(4) 0.5821(15) 0.7862(12) 0.047(6) Uani 0.50 1 d PDU . . H10F H 0.9545 0.6024 0.8369 0.057 Uiso 0.50 1 d PR . . C109 C 0.9407(6) 0.6131(15) 0.7239(9) 0.031(6) Uani 0.50 1 d PDU . . H10G H 0.9203 0.6514 0.7315 0.037 Uiso 0.50 1 d PR . . C110 C 0.9526(4) 0.5841(12) 0.6521(10) 0.035(5) Uani 0.50 1 d PDU . . H11A H 0.9396 0.6044 0.6085 0.041 Uiso 0.50 1 d PR . . 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 I1 0.0303(4) 0.0606(5) 0.0929(7) 0.0103(5) 0.0059(4) -0.0053(4) I2 0.0339(3) 0.0497(4) 0.0669(5) 0.0162(4) -0.0048(4) -0.0014(3) I3 0.0603(6) 0.1123(8) 0.0754(6) 0.0204(6) -0.0262(5) -0.0033(6) I4 0.0510(6) 0.0281(5) 0.0605(7) 0.000 0.000 0.0008(4) Cu1 0.0191(5) 0.0218(5) 0.0235(5) -0.0013(5) -0.0011(5) -0.0004(5) S1 0.0279(12) 0.0235(11) 0.0178(11) 0.0006(9) -0.0012(9) 0.0036(9) S2 0.0149(10) 0.0371(12) 0.0245(12) -0.0015(11) 0.0022(9) -0.0018(10) S3 0.0221(11) 0.0260(12) 0.0182(11) 0.0018(9) -0.0002(9) -0.0073(9) P1 0.0168(11) 0.0184(11) 0.0212(12) -0.0032(9) -0.0034(9) 0.0006(9) P2 0.0177(11) 0.0230(12) 0.0213(12) -0.0022(10) 0.0008(9) 0.0007(10) O1 0.023(3) 0.021(3) 0.032(4) 0.002(3) -0.015(3) -0.003(2) O2 0.020(3) 0.020(3) 0.012(3) 0.004(2) -0.003(2) -0.002(2) O3 0.017(3) 0.025(3) 0.031(3) -0.004(3) 0.007(3) 0.003(3) O4 0.013(3) 0.032(3) 0.019(3) -0.001(3) -0.001(2) 0.003(2) O5 0.020(3) 0.030(3) 0.024(3) -0.001(3) 0.008(3) -0.001(3) O6 0.019(3) 0.029(3) 0.017(3) -0.002(3) 0.006(2) 0.004(3) N1 0.027(4) 0.018(4) 0.032(5) -0.016(3) 0.006(3) -0.008(3) N2 0.017(4) 0.015(4) 0.031(4) -0.008(3) -0.008(3) -0.005(3) C1 0.017(5) 0.036(6) 0.024(5) -0.007(4) -0.007(4) -0.005(4) C2 0.029(5) 0.017(5) 0.022(5) 0.011(4) -0.006(4) 0.006(4) C3 0.026(5) 0.035(6) 0.026(5) -0.004(4) 0.008(4) 0.014(4) C4 0.038(5) 0.021(5) 0.014(4) -0.001(4) 0.000(4) -0.002(4) C5 0.040(6) 0.022(5) 0.018(5) 0.005(4) 0.006(4) 0.002(4) C6 0.061(7) 0.016(5) 0.024(5) -0.005(4) 0.001(5) 0.002(5) C7 0.037(5) 0.029(5) 0.022(5) 0.010(4) -0.010(4) -0.013(4) C8 0.038(5) 0.022(5) 0.015(4) -0.001(4) -0.013(4) -0.004(4) C9 0.037(5) 0.022(5) 0.016(4) 0.000(4) -0.014(4) -0.004(4) C10 0.016(4) 0.023(5) 0.018(4) 0.002(4) -0.001(3) 0.004(4) C11 0.023(5) 0.020(5) 0.017(5) -0.007(4) 0.000(4) 0.001(4) C12 0.030(5) 0.013(4) 0.037(6) -0.001(4) -0.009(4) 0.004(4) C13 0.026(5) 0.025(5) 0.030(5) 0.001(4) -0.002(4) -0.008(4) C14 0.009(4) 0.040(6) 0.051(6) 0.005(5) 0.000(4) -0.003(4) C15 0.027(5) 0.034(6) 0.054(7) -0.002(5) -0.012(5) 0.003(4) C16 0.027(6) 0.034(6) 0.057(7) 0.011(5) -0.018(5) 0.005(5) C17 0.032(5) 0.022(5) 0.040(6) -0.018(4) -0.014(4) -0.006(4) C18 0.026(5) 0.027(5) 0.025(5) -0.003(4) -0.007(4) -0.005(4) C19 0.030(5) 0.018(5) 0.014(4) -0.002(4) -0.003(4) 0.001(4) C20 0.005(4) 0.020(4) 0.022(5) -0.008(4) -0.005(3) -0.001(3) C21 0.020(4) 0.014(4) 0.030(5) -0.008(4) 0.002(4) -0.001(4) C22 0.025(5) 0.036(6) 0.024(5) 0.006(4) -0.007(4) -0.009(4) C23 0.029(5) 0.032(6) 0.049(6) 0.001(5) -0.003(5) -0.004(4) C24 0.028(5) 0.034(6) 0.043(6) -0.007(5) 0.011(5) 0.007(4) C25 0.035(6) 0.034(6) 0.056(7) -0.002(5) 0.017(5) 0.001(5) C26 0.035(6) 0.025(5) 0.074(8) 0.002(5) 0.027(6) 0.000(5) C27 0.032(6) 0.031(6) 0.057(7) -0.004(5) 0.020(5) -0.014(5) C28 0.018(5) 0.040(6) 0.053(7) -0.016(5) 0.010(4) -0.002(4) C29 0.019(4) 0.013(4) 0.029(5) -0.007(4) 0.004(4) -0.006(4) C30 0.021(5) 0.027(5) 0.019(5) 0.003(4) 0.002(4) 0.003(4) C31 0.011(4) 0.029(5) 0.014(4) -0.005(4) -0.004(3) -0.003(4) C32 0.016(4) 0.031(5) 0.019(5) 0.001(4) -0.010(4) -0.007(4) C33 0.006(4) 0.034(5) 0.028(5) -0.013(4) -0.001(4) 0.001(4) C34 0.013(4) 0.039(6) 0.037(6) -0.014(5) -0.004(4) -0.001(4) C35 0.019(5) 0.038(6) 0.028(5) 0.004(5) -0.009(4) 0.009(4) C36 0.018(5) 0.041(6) 0.031(5) 0.001(5) -0.012(4) -0.010(4) C37 0.028(5) 0.030(5) 0.019(5) 0.002(4) -0.015(4) -0.001(4) C38 0.015(4) 0.037(6) 0.020(5) -0.003(4) 0.004(4) 0.006(4) C39 0.018(4) 0.035(6) 0.023(5) 0.001(4) 0.001(4) -0.003(4) C40 0.014(4) 0.031(5) 0.022(5) -0.004(4) -0.007(4) 0.004(4) C41 0.029(5) 0.018(5) 0.020(5) 0.005(4) 0.003(4) -0.002(4) C42 0.018(4) 0.036(5) 0.016(4) 0.010(4) -0.004(4) -0.005(4) C43 0.033(5) 0.026(5) 0.025(5) 0.001(4) -0.005(4) -0.017(4) C44 0.032(5) 0.023(5) 0.016(5) 0.005(4) -0.005(4) -0.011(4) C45 0.037(6) 0.020(5) 0.030(5) 0.001(4) -0.005(4) -0.006(4) C46 0.052(7) 0.034(6) 0.014(5) 0.001(4) 0.008(4) -0.009(5) C47 0.051(7) 0.029(6) 0.024(5) -0.005(4) 0.010(5) 0.005(5) C48 0.022(5) 0.017(4) 0.025(5) 0.005(4) 0.004(4) -0.005(4) C49 0.037(5) 0.011(4) 0.020(4) 0.011(4) -0.008(4) -0.002(4) C50 0.019(4) 0.018(4) 0.015(4) 0.004(3) -0.006(3) -0.007(4) C51 0.022(5) 0.011(4) 0.025(5) 0.006(4) -0.003(4) -0.002(4) C52 0.015(4) 0.017(4) 0.020(5) -0.003(4) 0.004(4) 0.003(3) C53 0.014(4) 0.021(5) 0.036(5) -0.001(4) -0.005(4) -0.002(4) C54 0.035(6) 0.038(6) 0.034(6) -0.003(5) -0.006(4) 0.009(5) C55 0.020(5) 0.056(7) 0.037(6) 0.002(5) 0.007(4) -0.003(5) C56 0.030(5) 0.025(5) 0.027(5) 0.009(4) -0.001(4) -0.006(4) C57 0.024(5) 0.017(5) 0.027(5) -0.015(4) -0.002(4) 0.001(4) C58 0.029(5) 0.023(5) 0.026(5) -0.008(4) 0.014(4) 0.006(4) C59 0.023(5) 0.018(5) 0.027(5) 0.003(4) -0.002(4) 0.004(4) C60 0.034(5) 0.019(5) 0.013(4) 0.001(4) -0.002(4) 0.000(4) C61 0.041(6) 0.035(6) 0.029(6) -0.007(5) 0.013(5) -0.004(5) C62 0.071(9) 0.039(7) 0.038(7) 0.000(5) 0.024(6) -0.013(6) C63 0.045(8) 0.055(8) 0.076(10) -0.032(7) 0.033(7) -0.028(6) C64 0.024(6) 0.056(8) 0.083(10) -0.022(8) 0.007(6) -0.019(5) C65 0.016(5) 0.029(5) 0.050(6) -0.029(5) 0.003(4) -0.007(4) C66 0.044(6) 0.019(5) 0.043(6) -0.013(5) -0.022(5) -0.001(5) C67 0.027(6) 0.055(8) 0.071(9) -0.016(7) -0.037(6) 0.018(5) C68 0.069(10) 0.058(9) 0.103(13) -0.029(9) -0.054(10) 0.034(8) C69 0.086(10) 0.020(6) 0.050(7) -0.010(5) -0.027(7) 0.015(6) C70 0.043(6) 0.025(5) 0.056(7) -0.012(5) -0.022(6) 0.004(5) Cu2 0.0213(8) 0.0550(11) 0.0190(8) 0.000 0.000 -0.0028(8) P3 0.0196(12) 0.0436(15) 0.0216(12) -0.0004(11) 0.0030(10) 0.0084(11) S4 0.0243(12) 0.0334(13) 0.0304(13) -0.0026(10) -0.0009(10) 0.0084(10) S5 0.0169(17) 0.111(4) 0.0168(18) 0.000 0.000 0.011(2) O7 0.019(3) 0.048(4) 0.015(3) 0.001(3) 0.004(2) 0.004(3) O8 0.023(3) 0.056(5) 0.031(4) 0.006(3) 0.009(3) 0.019(3) O9 0.019(3) 0.043(4) 0.016(3) -0.004(3) -0.009(2) 0.013(3) C71 0.030(5) 0.024(5) 0.042(6) -0.001(4) 0.003(4) 0.000(4) C72 0.018(5) 0.044(6) 0.024(5) 0.004(4) 0.001(4) 0.011(4) C73 0.022(5) 0.035(6) 0.039(6) -0.007(5) 0.015(4) 0.007(4) C74 0.035(5) 0.016(5) 0.018(5) 0.002(4) -0.004(4) -0.001(4) C75 0.041(6) 0.022(5) 0.032(6) 0.002(4) 0.011(5) -0.002(4) C76 0.025(5) 0.038(6) 0.028(5) 0.005(4) -0.006(4) -0.006(4) C77 0.043(6) 0.033(6) 0.019(5) 0.005(4) -0.010(4) -0.003(5) C78 0.019(5) 0.043(6) 0.045(6) 0.000(5) -0.019(4) 0.009(4) C79 0.023(5) 0.021(5) 0.026(5) 0.003(4) -0.001(4) -0.007(4) C80 0.018(4) 0.026(5) 0.035(5) 0.009(4) 0.007(4) 0.001(4) C81 0.017(5) 0.034(5) 0.033(6) -0.001(4) -0.005(4) 0.015(4) C82 0.040(6) 0.032(6) 0.055(7) -0.018(5) -0.012(5) 0.017(5) C83 0.034(6) 0.036(6) 0.059(7) -0.011(6) -0.008(5) 0.013(5) C84 0.047(5) 0.046(5) 0.072(6) 0.003(5) -0.011(5) 0.010(5) C85 0.044(5) 0.046(5) 0.089(6) -0.013(5) -0.010(5) 0.010(4) C86 0.046(5) 0.045(5) 0.074(6) -0.026(5) -0.024(5) 0.014(4) C87 0.049(7) 0.046(7) 0.078(9) -0.028(7) -0.035(6) 0.039(6) C88 0.064(9) 0.091(11) 0.042(8) -0.009(8) -0.030(7) 0.065(8) C89 0.062(8) 0.055(8) 0.047(7) -0.017(6) -0.019(6) 0.037(7) C90 0.016(5) 0.048(7) 0.039(6) -0.011(5) -0.009(4) 0.020(5) C91 0.016(4) 0.038(6) 0.009(4) 0.002(4) -0.004(3) 0.011(4) C92 0.017(4) 0.041(6) 0.020(5) -0.001(4) -0.004(4) -0.004(4) C93 0.026(5) 0.042(6) 0.022(5) -0.001(4) 0.000(4) 0.003(4) C94 0.023(5) 0.039(6) 0.027(5) -0.009(5) -0.010(4) -0.005(4) C95 0.037(5) 0.041(6) 0.020(5) 0.000(4) -0.005(4) -0.008(5) C96 0.078(9) 0.037(7) 0.053(7) 0.013(6) -0.042(7) -0.008(6) C97 0.042(7) 0.060(8) 0.053(8) 0.023(6) -0.025(6) -0.029(6) C98 0.034(6) 0.070(8) 0.022(5) 0.028(5) -0.007(4) -0.025(6) C99 0.008(4) 0.053(6) 0.022(5) 0.003(5) -0.005(4) -0.014(4) C100 0.010(4) 0.061(7) 0.025(5) -0.008(5) 0.004(4) -0.018(4) N3 0.030(5) 0.030(5) 0.026(5) 0.003(4) 0.001(4) 0.000(4) N4 0.042(6) 0.036(6) 0.039(6) 0.009(5) 0.000(5) -0.001(4) C101 0.024(5) 0.025(6) 0.020(5) 0.003(4) -0.004(4) -0.001(4) C102 0.043(6) 0.043(6) 0.044(7) 0.004(5) 0.001(5) -0.002(5) C103 0.038(6) 0.039(6) 0.036(6) 0.000(5) -0.002(5) 0.004(5) C104 0.024(6) 0.026(6) 0.022(6) -0.005(5) -0.002(5) -0.002(5) C105 0.025(6) 0.022(6) 0.025(6) -0.002(4) -0.004(4) -0.004(4) C106 0.026(4) 0.023(4) 0.017(4) 0.000 0.000 0.000(4) C107 0.033(6) 0.034(6) 0.028(6) -0.003(4) 0.004(4) -0.002(4) C108 0.048(7) 0.048(7) 0.047(7) 0.000(5) 0.008(5) 0.001(5) C109 0.030(7) 0.032(7) 0.031(7) 0.002(5) 0.001(5) -0.001(5) C110 0.033(6) 0.034(6) 0.036(6) 0.005(5) -0.001(5) 0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 I2 2.8388(13) . ? I2 I3 2.8613(15) . ? Cu1 N2 2.045(7) . ? Cu1 N1 2.061(7) . ? Cu1 P1 2.220(2) . ? Cu1 P2 2.223(2) . ? S1 C10 1.752(8) . ? S1 C11 1.768(9) . ? S2 C31 1.781(8) . ? S2 C30 1.789(9) . ? S3 C50 1.782(8) . ? S3 C51 1.785(8) . ? P1 O1 1.590(6) . ? P1 O2 1.618(6) . ? P1 O3 1.627(6) . ? P2 O4 1.605(6) . ? P2 O5 1.606(6) . ? P2 O6 1.621(6) . ? O1 C1 1.393(10) . ? O2 C20 1.375(9) . ? O3 C21 1.384(10) . ? O4 C40 1.420(10) . ? O5 C41 1.409(10) . ? O6 C60 1.411(10) . ? N1 C61 1.330(12) . ? N1 C65 1.343(12) . ? N2 C70 1.314(13) . ? N2 C66 1.330(12) . ? C1 C2 1.388(12) . ? C1 C10 1.398(11) . ? C2 C3 1.360(13) . ? C2 H2 0.9500 . ? C3 C4 1.421(13) . ? C3 H3 0.9500 . ? C4 C9 1.405(13) . ? C4 C5 1.414(12) . ? C5 C6 1.359(13) . ? C5 H5 0.9500 . ? C6 C7 1.415(13) . ? C6 H6 0.9500 . ? C7 C8 1.370(13) . ? C7 H7 0.9500 . ? C8 C9 1.448(13) . ? C8 H8 0.9500 . ? C9 C10 1.416(12) . ? C11 C20 1.375(11) . ? C11 C12 1.427(12) . ? C12 C13 1.436(13) . ? C12 C17 1.451(13) . ? C13 C14 1.357(12) . ? C13 H13 0.9500 . ? C14 C15 1.400(14) . ? C14 H14 0.9500 . ? C15 C16 1.374(15) . ? C15 H15 0.9500 . ? C16 C17 1.426(13) . ? C16 H16 0.9500 . ? C17 C18 1.395(13) . ? C18 C19 1.345(12) . ? C18 H18 0.9500 . ? C19 C20 1.417(11) . ? C19 H19 0.9500 . ? C21 C30 1.376(12) . ? C21 C22 1.384(12) . ? C22 C23 1.362(13) . ? C22 H22 0.9500 . ? C23 C24 1.429(14) . ? C23 H23 0.9500 . ? C24 C25 1.386(14) . ? C24 C29 1.427(13) . ? C25 C26 1.366(15) . ? C25 H25 0.9500 . ? C26 C27 1.398(16) . ? C26 H26 0.9500 . ? C27 C28 1.378(14) . ? C27 H27 0.9500 . ? C28 C29 1.427(12) . ? C28 H28 0.9500 . ? C29 C30 1.426(12) . ? C31 C40 1.354(12) . ? C31 C32 1.440(12) . ? C32 C33 1.411(12) . ? C32 C37 1.434(12) . ? C33 C34 1.369(13) . ? C33 H33 0.9500 . ? C34 C35 1.415(13) . ? C34 H34 0.9500 . ? C35 C36 1.318(13) . ? C35 H35 0.9500 . ? C36 C37 1.428(13) . ? C36 H36 0.9500 . ? C37 C38 1.435(12) . ? C38 C39 1.349(13) . ? C38 H38 0.9500 . ? C39 C40 1.394(12) . ? C39 H39 0.9500 . ? C41 C50 1.373(12) . ? C41 C42 1.413(12) . ? C42 C43 1.368(12) . ? C42 H42 0.9500 . ? C43 C44 1.424(13) . ? C43 H43 0.9500 . ? C44 C45 1.409(12) . ? C44 C49 1.441(12) . ? C45 C46 1.375(13) . ? C45 H45 0.9500 . ? C46 C47 1.413(14) . ? C46 H46 0.9500 . ? C47 C48 1.347(12) . ? C47 H47 0.9500 . ? C48 C49 1.393(12) . ? C48 H48 0.9500 . ? C49 C50 1.431(11) . ? C51 C60 1.382(12) . ? C51 C52 1.448(11) . ? C52 C53 1.368(12) . ? C52 C57 1.433(12) . ? C53 C54 1.354(13) . ? C53 H53 0.9500 . ? C54 C55 1.422(14) . ? C54 H54 0.9500 . ? C55 C56 1.347(13) . ? C55 H55 0.9500 . ? C56 C57 1.397(12) . ? C56 H56 0.9500 . ? C57 C58 1.434(13) . ? C58 C59 1.358(12) . ? C58 H58 0.9500 . ? C59 C60 1.394(12) . ? C59 H59 0.9500 . ? C61 C62 1.385(14) . ? C61 H61 0.9500 . ? C62 C63 1.396(18) . ? C62 H62 0.9500 . ? C63 C64 1.389(18) . ? C63 H63 0.9500 . ? C64 C65 1.398(14) . ? C64 H64 0.9500 . ? C65 C66 1.459(13) . ? C66 C67 1.432(13) . ? C67 C68 1.34(2) . ? C67 H67 0.9500 . ? C68 C69 1.39(2) . ? C68 H68 0.9500 . ? C69 C70 1.375(15) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? Cu2 N4 2.040(7) . ? Cu2 N3 2.063(6) . ? Cu2 P3 2.194(3) 2_765 ? Cu2 P3 2.194(3) . ? P3 O8 1.612(7) . ? P3 O9 1.619(6) . ? P3 O7 1.632(6) . ? S4 C80 1.762(8) . ? S4 C81 1.765(9) . ? S5 C100 1.786(9) 2_765 ? S5 C100 1.786(9) . ? O7 C71 1.387(11) . ? O8 C90 1.390(12) . ? O9 C91 1.384(10) . ? C71 C72 1.398(12) . ? C71 C80 1.408(13) . ? C72 C73 1.353(12) . ? C72 H72 0.9500 . ? C73 C74 1.416(13) . ? C73 H73 0.9500 . ? C74 C75 1.395(13) . ? C74 C79 1.458(12) . ? C75 C76 1.341(13) . ? C75 H75 0.9500 . ? C76 C77 1.429(13) . ? C76 H76 0.9500 . ? C77 C78 1.349(13) . ? C77 H77 0.9500 . ? C78 C79 1.415(12) . ? C78 H78 0.9500 . ? C79 C80 1.437(13) . ? C81 C90 1.354(13) . ? C81 C82 1.444(14) . ? C82 C83 1.411(15) . ? C82 C87 1.450(15) . ? C83 C84 1.444(16) . ? C83 H83 0.9500 . ? C84 C85 1.430(17) . ? C84 H84 0.9500 . ? C85 C86 1.283(17) . ? C85 H85 0.9500 . ? C86 C87 1.429(18) . ? C86 H86 0.9500 . ? C87 C88 1.409(18) . ? C88 C89 1.335(18) . ? C88 H88 0.9500 . ? C89 C90 1.397(14) . ? C89 H89 0.9500 . ? C91 C100 1.378(12) . ? C91 C92 1.441(12) . ? C92 C93 1.380(13) . ? C92 H92 0.9500 . ? C93 C94 1.389(13) . ? C93 H93 0.9500 . ? C94 C95 1.403(14) . ? C94 C99 1.420(13) . ? C95 C96 1.389(15) . ? C95 H95 0.9500 . ? C96 C97 1.398(18) . ? C96 H96 0.9500 . ? C97 C98 1.309(16) . ? C97 H97 0.9500 . ? C98 C99 1.452(13) . ? C98 H98 0.9500 . ? C99 C100 1.401(14) . ? N3 C105 1.338(11) . ? N3 C101 1.346(11) . ? N4 C110 1.320(11) . ? N4 C106 1.336(10) . ? C101 C102 1.391(12) . ? C101 H10A 0.9602 . ? C102 C103 1.394(12) . ? C102 H10B 0.9598 . ? C103 C104 1.401(12) . ? C103 H10C 0.9601 . ? C104 C105 1.405(12) . ? C104 H10D 0.9599 . ? C105 C106 1.466(11) . ? C106 C107 1.403(11) . ? C107 C108 1.390(12) . ? C107 H10E 0.9600 . ? C108 C109 1.399(12) . ? C108 H10F 0.9599 . ? C109 C110 1.403(12) . ? C109 H10G 0.9603 . ? C110 H11A 0.9599 . ? 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 I1 I2 I3 178.67(4) . . ? N2 Cu1 N1 81.1(3) . . ? N2 Cu1 P1 112.2(2) . . ? N1 Cu1 P1 113.0(2) . . ? N2 Cu1 P2 114.7(2) . . ? N1 Cu1 P2 115.2(2) . . ? P1 Cu1 P2 115.88(8) . . ? C10 S1 C11 102.3(4) . . ? C31 S2 C30 105.4(4) . . ? C50 S3 C51 102.4(4) . . ? O1 P1 O2 101.8(3) . . ? O1 P1 O3 97.1(3) . . ? O2 P1 O3 97.9(3) . . ? O1 P1 Cu1 123.7(3) . . ? O2 P1 Cu1 117.7(2) . . ? O3 P1 Cu1 114.0(2) . . ? O4 P2 O5 96.1(3) . . ? O4 P2 O6 98.6(3) . . ? O5 P2 O6 102.4(3) . . ? O4 P2 Cu1 115.9(2) . . ? O5 P2 Cu1 122.7(2) . . ? O6 P2 Cu1 116.7(2) . . ? C1 O1 P1 123.7(5) . . ? C20 O2 P1 123.2(5) . . ? C21 O3 P1 120.4(5) . . ? C40 O4 P2 119.5(5) . . ? C41 O5 P2 121.1(5) . . ? C60 O6 P2 121.5(5) . . ? C61 N1 C65 121.1(8) . . ? C61 N1 Cu1 126.7(7) . . ? C65 N1 Cu1 112.0(6) . . ? C70 N2 C66 118.8(8) . . ? C70 N2 Cu1 128.1(7) . . ? C66 N2 Cu1 112.9(6) . . ? C2 C1 O1 118.3(7) . . ? C2 C1 C10 122.1(8) . . ? O1 C1 C10 119.6(8) . . ? C3 C2 C1 120.4(9) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 120.4(8) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C9 C4 C5 120.5(8) . . ? C9 C4 C3 118.6(8) . . ? C5 C4 C3 120.8(8) . . ? C6 C5 C4 120.8(9) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.7(8) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C7 C6 121.4(9) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 119.6(9) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C4 C9 C10 121.2(8) . . ? C4 C9 C8 118.0(8) . . ? C10 C9 C8 120.8(8) . . ? C1 C10 C9 117.2(8) . . ? C1 C10 S1 118.2(7) . . ? C9 C10 S1 124.6(7) . . ? C20 C11 C12 119.3(8) . . ? C20 C11 S1 121.2(6) . . ? C12 C11 S1 119.3(7) . . ? C11 C12 C13 123.7(8) . . ? C11 C12 C17 118.8(8) . . ? C13 C12 C17 117.4(8) . . ? C14 C13 C12 121.8(9) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 119.9(9) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 122.1(9) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C17 119.5(9) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 122.5(9) . . ? C18 C17 C12 118.3(8) . . ? C16 C17 C12 119.2(9) . . ? C19 C18 C17 122.1(9) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 120.3(8) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? O2 C20 C11 123.1(7) . . ? O2 C20 C19 116.1(7) . . ? C11 C20 C19 120.8(7) . . ? C30 C21 O3 118.0(8) . . ? C30 C21 C22 121.4(8) . . ? O3 C21 C22 120.5(8) . . ? C23 C22 C21 120.5(9) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 121.4(9) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C29 118.9(9) . . ? C25 C24 C23 123.6(10) . . ? C29 C24 C23 117.5(9) . . ? C26 C25 C24 121.9(11) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C25 C26 C27 121.7(10) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 117.0(10) . . ? C28 C27 H27 121.5 . . ? C26 C27 H27 121.5 . . ? C27 C28 C29 123.5(10) . . ? C27 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C24 C29 C30 119.6(8) . . ? C24 C29 C28 116.8(8) . . ? C30 C29 C28 123.6(9) . . ? C21 C30 C29 119.5(8) . . ? C21 C30 S2 122.6(7) . . ? C29 C30 S2 117.4(7) . . ? C40 C31 C32 119.6(8) . . ? C40 C31 S2 123.1(7) . . ? C32 C31 S2 117.0(6) . . ? C33 C32 C37 118.8(8) . . ? C33 C32 C31 123.9(8) . . ? C37 C32 C31 117.3(8) . . ? C34 C33 C32 120.3(8) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 119.9(8) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 121.5(9) . . ? C36 C35 H35 119.2 . . ? C34 C35 H35 119.2 . . ? C35 C36 C37 121.0(9) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C36 C37 C32 118.0(8) . . ? C36 C37 C38 121.8(8) . . ? C32 C37 C38 120.2(8) . . ? C39 C38 C37 119.2(8) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 121.0(8) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C31 C40 C39 122.5(8) . . ? C31 C40 O4 118.5(8) . . ? C39 C40 O4 118.8(7) . . ? C50 C41 O5 119.3(7) . . ? C50 C41 C42 123.4(8) . . ? O5 C41 C42 117.2(7) . . ? C43 C42 C41 117.5(8) . . ? C43 C42 H42 121.3 . . ? C41 C42 H42 121.3 . . ? C42 C43 C44 122.1(8) . . ? C42 C43 H43 119.0 . . ? C44 C43 H43 119.0 . . ? C45 C44 C43 122.3(8) . . ? C45 C44 C49 118.0(8) . . ? C43 C44 C49 119.8(8) . . ? C46 C45 C44 122.7(9) . . ? C46 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? C45 C46 C47 117.7(9) . . ? C45 C46 H46 121.2 . . ? C47 C46 H46 121.2 . . ? C48 C47 C46 121.1(10) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C47 C48 C49 122.6(9) . . ? C47 C48 H48 118.7 . . ? C49 C48 H48 118.7 . . ? C48 C49 C50 125.1(8) . . ? C48 C49 C44 117.8(8) . . ? C50 C49 C44 117.1(8) . . ? C41 C50 C49 120.1(7) . . ? C41 C50 S3 119.3(6) . . ? C49 C50 S3 120.7(6) . . ? C60 C51 C52 119.9(7) . . ? C60 C51 S3 122.4(6) . . ? C52 C51 S3 117.5(6) . . ? C53 C52 C57 119.3(8) . . ? C53 C52 C51 124.4(8) . . ? C57 C52 C51 116.3(7) . . ? C54 C53 C52 121.5(9) . . ? C54 C53 H53 119.3 . . ? C52 C53 H53 119.3 . . ? C53 C54 C55 119.9(9) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 119.4(9) . . ? C56 C55 H55 120.3 . . ? C54 C55 H55 120.3 . . ? C55 C56 C57 121.7(9) . . ? C55 C56 H56 119.2 . . ? C57 C56 H56 119.2 . . ? C56 C57 C58 121.1(8) . . ? C56 C57 C52 118.0(8) . . ? C58 C57 C52 120.9(8) . . ? C59 C58 C57 120.3(9) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C58 C59 C60 119.7(8) . . ? C58 C59 H59 120.2 . . ? C60 C59 H59 120.1 . . ? C51 C60 C59 122.4(8) . . ? C51 C60 O6 121.0(7) . . ? C59 C60 O6 116.4(7) . . ? N1 C61 C62 121.6(11) . . ? N1 C61 H61 119.2 . . ? C62 C61 H61 119.2 . . ? C61 C62 C63 119.9(11) . . ? C61 C62 H62 120.1 . . ? C63 C62 H62 120.1 . . ? C64 C63 C62 116.7(10) . . ? C64 C63 H63 121.7 . . ? C62 C63 H63 121.7 . . ? C63 C64 C65 121.7(11) . . ? C63 C64 H64 119.2 . . ? C65 C64 H64 119.2 . . ? N1 C65 C64 119.0(10) . . ? N1 C65 C66 116.7(9) . . ? C64 C65 C66 124.3(10) . . ? N2 C66 C67 120.8(10) . . ? N2 C66 C65 117.0(9) . . ? C67 C66 C65 122.2(11) . . ? C68 C67 C66 117.0(12) . . ? C68 C67 H67 121.5 . . ? C66 C67 H67 121.5 . . ? C67 C68 C69 123.2(12) . . ? C67 C68 H68 118.4 . . ? C69 C68 H68 118.4 . . ? C70 C69 C68 114.2(12) . . ? C70 C69 H69 122.9 . . ? C68 C69 H69 122.9 . . ? N2 C70 C69 125.8(11) . . ? N2 C70 H70 117.1 . . ? C69 C70 H70 117.1 . . ? N4 Cu2 N3 79.2(5) . . ? N4 Cu2 P3 115.5(4) . 2_765 ? N3 Cu2 P3 114.6(4) . 2_765 ? N4 Cu2 P3 117.4(4) . . ? N3 Cu2 P3 99.1(4) . . ? P3 Cu2 P3 121.08(14) 2_765 . ? O8 P3 O9 98.1(3) . . ? O8 P3 O7 101.8(4) . . ? O9 P3 O7 97.3(3) . . ? O8 P3 Cu2 120.9(3) . . ? O9 P3 Cu2 118.6(3) . . ? O7 P3 Cu2 116.0(2) . . ? C80 S4 C81 104.2(4) . . ? C100 S5 C100 107.8(6) 2_765 . ? C71 O7 P3 122.2(6) . . ? C90 O8 P3 120.1(5) . . ? C91 O9 P3 115.7(5) . . ? O7 C71 C72 117.2(8) . . ? O7 C71 C80 121.0(8) . . ? C72 C71 C80 121.8(9) . . ? C73 C72 C71 120.4(9) . . ? C73 C72 H72 119.8 . . ? C71 C72 H72 119.8 . . ? C72 C73 C74 122.2(8) . . ? C72 C73 H73 118.9 . . ? C74 C73 H73 118.9 . . ? C75 C74 C73 123.4(8) . . ? C75 C74 C79 118.6(8) . . ? C73 C74 C79 117.8(8) . . ? C76 C75 C74 122.6(9) . . ? C76 C75 H75 118.7 . . ? C74 C75 H75 118.7 . . ? C75 C76 C77 118.9(9) . . ? C75 C76 H76 120.5 . . ? C77 C76 H76 120.5 . . ? C78 C77 C76 121.2(9) . . ? C78 C77 H77 119.4 . . ? C76 C77 H77 119.4 . . ? C77 C78 C79 121.0(9) . . ? C77 C78 H78 119.5 . . ? C79 C78 H78 119.5 . . ? C78 C79 C80 122.9(8) . . ? C78 C79 C74 117.4(8) . . ? C80 C79 C74 119.6(8) . . ? C71 C80 C79 117.8(8) . . ? C71 C80 S4 123.8(7) . . ? C79 C80 S4 118.2(7) . . ? C90 C81 C82 117.8(9) . . ? C90 C81 S4 120.1(8) . . ? C82 C81 S4 122.1(7) . . ? C83 C82 C81 121.7(9) . . ? C83 C82 C87 121.2(10) . . ? C81 C82 C87 117.1(11) . . ? C82 C83 C84 120.2(10) . . ? C82 C83 H83 119.9 . . ? C84 C83 H83 119.9 . . ? C85 C84 C83 115.5(12) . . ? C85 C84 H84 122.3 . . ? C83 C84 H84 122.3 . . ? C86 C85 C84 124.3(12) . . ? C86 C85 H85 117.9 . . ? C84 C85 H85 117.9 . . ? C85 C86 C87 123.9(12) . . ? C85 C86 H86 118.0 . . ? C87 C86 H86 118.0 . . ? C88 C87 C86 124.6(12) . . ? C88 C87 C82 120.4(12) . . ? C86 C87 C82 114.9(13) . . ? C89 C88 C87 120.5(12) . . ? C89 C88 H88 119.8 . . ? C87 C88 H88 119.8 . . ? C88 C89 C90 119.5(13) . . ? C88 C89 H89 120.3 . . ? C90 C89 H89 120.3 . . ? C81 C90 O8 118.3(8) . . ? C81 C90 C89 124.5(11) . . ? O8 C90 C89 117.2(10) . . ? C100 C91 O9 122.1(8) . . ? C100 C91 C92 120.7(8) . . ? O9 C91 C92 117.2(8) . . ? C93 C92 C91 118.6(8) . . ? C93 C92 H92 120.7 . . ? C91 C92 H92 120.7 . . ? C92 C93 C94 121.3(9) . . ? C92 C93 H93 119.3 . . ? C94 C93 H93 119.3 . . ? C93 C94 C95 120.1(9) . . ? C93 C94 C99 119.7(9) . . ? C95 C94 C99 120.1(9) . . ? C96 C95 C94 119.6(10) . . ? C96 C95 H95 120.2 . . ? C94 C95 H95 120.2 . . ? C95 C96 C97 121.8(11) . . ? C95 C96 H96 119.1 . . ? C97 C96 H96 119.1 . . ? C98 C97 C96 118.0(11) . . ? C98 C97 H97 121.0 . . ? C96 C97 H97 121.0 . . ? C97 C98 C99 125.2(11) . . ? C97 C98 H98 117.4 . . ? C99 C98 H98 117.4 . . ? C100 C99 C94 119.9(8) . . ? C100 C99 C98 124.9(9) . . ? C94 C99 C98 115.2(9) . . ? C91 C100 C99 119.8(8) . . ? C91 C100 S5 120.0(8) . . ? C99 C100 S5 119.1(7) . . ? C105 N3 C101 115.5(9) . . ? C105 N3 Cu2 114.8(8) . . ? C101 N3 Cu2 129.6(9) . . ? C110 N4 C106 124.4(10) . . ? C110 N4 Cu2 120.6(10) . . ? C106 N4 Cu2 114.6(7) . . ? N3 C101 C102 125.0(14) . . ? N3 C101 H10A 118.8 . . ? C102 C101 H10A 116.2 . . ? C101 C102 C103 116.6(17) . . ? C101 C102 H10B 123.9 . . ? C103 C102 H10B 119.5 . . ? C102 C103 C104 121.5(19) . . ? C102 C103 H10C 119.6 . . ? C104 C103 H10C 118.9 . . ? C105 C104 C103 114.9(17) . . ? C105 C104 H10D 123.1 . . ? C103 C104 H10D 122.0 . . ? N3 C105 C104 126.2(12) . . ? N3 C105 C106 114.6(10) . . ? C104 C105 C106 119.2(12) . . ? N4 C106 C107 117.5(8) . . ? N4 C106 C105 116.1(9) . . ? C107 C106 C105 126.2(10) . . ? C108 C107 C106 119.5(15) . . ? C108 C107 H10E 120.8 . . ? C106 C107 H10E 119.7 . . ? C107 C108 C109 121(2) . . ? C107 C108 H10F 118.0 . . ? C109 C108 H10F 120.7 . . ? C110 C109 C108 116(2) . . ? C110 C109 H10G 123.5 . . ? C108 C109 H10G 120.5 . . ? N4 C110 C109 121.3(17) . . ? N4 C110 H11A 121.1 . . ? C109 C110 H11A 117.6 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.82 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.801 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.109