# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Ventura, Barbara' 'Maini, Lucia' 'Braga, Dario' 'Mazzeo, Paolo' _publ_contact_author_name 'Dr Barbara Ventura, ' _publ_contact_author_email l.maini@unibo.it _publ_section_title ; Polymorph and isomer conversion of complexes based on CuI and PPh3 easily observed via luminescence ; _publ_requested_category FM # Attachment '- 1a_90K.cif' data_shelxl1 _database_code_depnum_ccdc_archive 'CCDC 838119' #TrackingRef '- 1a_90K.cif' _audit_update_record ; 2011-06-28 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _chemical_formula_weight 1811.85 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_cell_setting monoclinic 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 13.4237(10) _cell_length_b 26.406(3) _cell_length_c 19.4266(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.531(7) _cell_angle_gamma 90.00 _cell_volume 6791.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 13001 _cell_measurement_theta_min 2.7734 _cell_measurement_theta_max 29.1157 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3524 _exptl_absorpt_coefficient_mu 3.189 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 90(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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35458 _diffrn_reflns_av_R_equivalents 0.0998 _diffrn_reflns_av_sigmaI/netI 0.0921 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 29.18 _reflns_number_total 15590 _reflns_number_gt 12905 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00004(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15590 _refine_ls_number_parameters 758 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 C25 C 0.2394(3) 0.02208(16) 0.5593(2) 0.0127(9) Uani 1 1 d . . . C1 C 0.6155(3) 0.00994(17) 0.7385(2) 0.0149(9) Uani 1 1 d . . . C20 C 0.0376(3) 0.05215(18) 0.6973(3) 0.0206(11) Uani 1 1 d . . . H20 H 0.0522 0.0857 0.7094 0.025 Uiso 1 1 calc R . . C4 C 0.6022(3) -0.08517(18) 0.6733(3) 0.0211(11) Uani 1 1 d . . . H4 H 0.5982 -0.1169 0.6522 0.025 Uiso 1 1 calc R . . C28 C 0.3384(4) -0.04595(19) 0.4834(3) 0.0228(11) Uani 1 1 d . . . H28 H 0.3715 -0.0681 0.4576 0.027 Uiso 1 1 calc R . . C31 C 0.1005(3) 0.10454(17) 0.5442(3) 0.0184(10) Uani 1 1 d . . . C13 C 0.6591(3) 0.05012(17) 0.8754(2) 0.0169(10) Uani 1 1 d . . . C2 C 0.6846(3) -0.00483(18) 0.6960(3) 0.0194(10) Uani 1 1 d . . . H2 H 0.7363 0.0171 0.6894 0.023 Uiso 1 1 calc R . . C37 C 0.1513(3) 0.13211(17) 0.9527(3) 0.0186(10) Uani 1 1 d . . . C30 C 0.3381(3) 0.00630(17) 0.5845(2) 0.0160(10) Uani 1 1 d . . . H30 H 0.3710 0.0182 0.6274 0.019 Uiso 1 1 calc R . . C24 C 0.0669(3) -0.02232(17) 0.6322(2) 0.0161(10) Uani 1 1 d . . . H24 H 0.0999 -0.0387 0.6001 0.019 Uiso 1 1 calc R . . C8 C 0.7306(3) 0.11679(17) 0.6937(3) 0.0184(10) Uani 1 1 d . . . H8 H 0.6776 0.1067 0.6593 0.022 Uiso 1 1 calc R . . C23 C -0.0028(3) -0.04840(18) 0.6640(3) 0.0217(11) Uani 1 1 d . . . H23 H -0.0161 -0.0823 0.6534 0.026 Uiso 1 1 calc R . . C3 C 0.6773(3) -0.05194(18) 0.6632(3) 0.0208(11) Uani 1 1 d . . . H3 H 0.7234 -0.0609 0.6345 0.025 Uiso 1 1 calc R . . C10 C 0.8076(3) 0.12123(16) 0.8143(3) 0.0202(11) Uani 1 1 d . . . H10 H 0.8081 0.1132 0.8610 0.024 Uiso 1 1 calc R . . C29 C 0.3881(4) -0.02721(19) 0.5460(3) 0.0247(11) Uani 1 1 d . . . H29 H 0.4544 -0.0368 0.5626 0.030 Uiso 1 1 calc R . . C7 C 0.7289(3) 0.10423(16) 0.7635(3) 0.0148(9) Uani 1 1 d . . . C33 C -0.0598(4) 0.1350(2) 0.4839(3) 0.0284(13) Uani 1 1 d . . . H33 H -0.1300 0.1343 0.4768 0.034 Uiso 1 1 calc R . . C9 C 0.8106(4) 0.14429(17) 0.6751(3) 0.0220(11) Uani 1 1 d . . . H9 H 0.8120 0.1514 0.6284 0.026 Uiso 1 1 calc R . . C32 C -0.0054(3) 0.10400(18) 0.5337(3) 0.0213(11) Uani 1 1 d . . . H32 H -0.0390 0.0827 0.5603 0.026 Uiso 1 1 calc R . . C27 C 0.2393(4) -0.03205(19) 0.4587(3) 0.0254(11) Uani 1 1 d . . . H27 H 0.2056 -0.0458 0.4172 0.030 Uiso 1 1 calc R . . C19 C 0.0874(3) 0.02876(16) 0.6485(2) 0.0134(9) Uani 1 1 d . . . C5 C 0.5335(4) -0.07118(18) 0.7146(3) 0.0221(11) Uani 1 1 d . . . H5 H 0.4819 -0.0935 0.7205 0.026 Uiso 1 1 calc R . . C26 C 0.1905(3) 0.00198(17) 0.4954(2) 0.0174(10) Uani 1 1 d . . . H26 H 0.1246 0.0118 0.4778 0.021 Uiso 1 1 calc R . . C17 C 0.7597(4) -0.00443(18) 0.9602(3) 0.0237(12) Uani 1 1 d . . . H17 H 0.8073 -0.0300 0.9709 0.028 Uiso 1 1 calc R . . C42 C 0.1082(3) 0.09686(19) 0.9023(3) 0.0220(11) Uani 1 1 d . . . H42 H 0.1307 0.0947 0.8596 0.026 Uiso 1 1 calc R . . C34 C 0.1482(4) 0.1380(2) 0.5049(3) 0.0300(13) Uani 1 1 d . . . H34 H 0.2184 0.1398 0.5124 0.036 Uiso 1 1 calc R . . C22 C -0.0525(3) -0.02419(19) 0.7116(3) 0.0226(11) Uani 1 1 d . . . H22 H -0.0992 -0.0420 0.7326 0.027 Uiso 1 1 calc R . . C40 C -0.0042(4) 0.06934(19) 0.9784(3) 0.0286(13) Uani 1 1 d . . . H40 H -0.0574 0.0489 0.9866 0.034 Uiso 1 1 calc R . . C41 C 0.0315(4) 0.06515(19) 0.9171(3) 0.0274(12) Uani 1 1 d . . . H41 H 0.0045 0.0408 0.8847 0.033 Uiso 1 1 calc R . . C35 C 0.0930(4) 0.16879(19) 0.4551(3) 0.0314(14) Uani 1 1 d . . . H35 H 0.1258 0.1906 0.4286 0.038 Uiso 1 1 calc R . . C6 C 0.5392(3) -0.02414(18) 0.7480(3) 0.0218(11) Uani 1 1 d . . . H6 H 0.4925 -0.0155 0.7765 0.026 Uiso 1 1 calc R . . C11 C 0.8851(4) 0.15011(18) 0.7954(3) 0.0266(12) Uani 1 1 d . . . H11 H 0.9359 0.1623 0.8298 0.032 Uiso 1 1 calc R . . C16 C 0.7306(3) 0.01125(17) 0.8916(3) 0.0178(10) Uani 1 1 d . . . H16 H 0.7587 -0.0041 0.8561 0.021 Uiso 1 1 calc R . . C14 C 0.6164(4) 0.0724(2) 0.9284(3) 0.0289(12) Uani 1 1 d . . . H14 H 0.5684 0.0979 0.9183 0.035 Uiso 1 1 calc R . . C15 C 0.6463(5) 0.0560(2) 0.9975(3) 0.0368(14) Uani 1 1 d . . . H15 H 0.6180 0.0707 1.0333 0.044 Uiso 1 1 calc R . . C21 C -0.0334(3) 0.02630(19) 0.7282(3) 0.0229(11) Uani 1 1 d . . . H21 H -0.0678 0.0426 0.7597 0.028 Uiso 1 1 calc R . . C38 C 0.1145(4) 0.13518(19) 1.0151(3) 0.0324(14) Uani 1 1 d . . . H38 H 0.1418 0.1587 1.0486 0.039 Uiso 1 1 calc R . . C39 C 0.0374(4) 0.1035(2) 1.0281(3) 0.0348(14) Uani 1 1 d . . . H39 H 0.0139 0.1054 1.0704 0.042 Uiso 1 1 calc R . . C43 C 0.3489(3) 0.17151(18) 1.0058(2) 0.0165(10) Uani 1 1 d . . . C50 C 0.1343(4) 0.26058(18) 0.8837(3) 0.0242(11) Uani 1 1 d . . . H50 H 0.1337 0.2458 0.8402 0.029 Uiso 1 1 calc R . . C49 C 0.1892(3) 0.23773(17) 0.9426(3) 0.0177(10) Uani 1 1 d . . . C44 C 0.4138(3) 0.2131(2) 1.0250(3) 0.0238(11) Uani 1 1 d . . . H44 H 0.4028 0.2434 1.0006 0.029 Uiso 1 1 calc R . . C12 C 0.8880(3) 0.16105(18) 0.7262(3) 0.0258(12) Uani 1 1 d . . . H12 H 0.9414 0.1795 0.7141 0.031 Uiso 1 1 calc R . . C45 C 0.3696(4) 0.1258(2) 1.0413(3) 0.0259(12) Uani 1 1 d . . . H45 H 0.3288 0.0978 1.0287 0.031 Uiso 1 1 calc R . . C36 C -0.0112(4) 0.16692(18) 0.4447(3) 0.0297(13) Uani 1 1 d . . . H36 H -0.0486 0.1874 0.4110 0.036 Uiso 1 1 calc R . . C51 C 0.1904(3) 0.26113(17) 1.0068(3) 0.0197(10) Uani 1 1 d . . . H51 H 0.2267 0.2467 1.0469 0.024 Uiso 1 1 calc R . . C18 C 0.7176(4) 0.0182(2) 1.0124(3) 0.0318(13) Uani 1 1 d . . . H18 H 0.7374 0.0079 1.0584 0.038 Uiso 1 1 calc R . . C61 C 0.5405(3) 0.30263(17) 0.6875(3) 0.0160(10) Uani 1 1 d . . . C55 C 0.3628(3) 0.28784(16) 0.5817(2) 0.0140(9) Uani 1 1 d . . . C66 C 0.5744(4) 0.35223(19) 0.6997(3) 0.0272(12) Uani 1 1 d . . . H66 H 0.5282 0.3783 0.7014 0.033 Uiso 1 1 calc R . . C63 C 0.7144(3) 0.27500(19) 0.6948(3) 0.0255(12) Uani 1 1 d . . . H63 H 0.7610 0.2491 0.6937 0.031 Uiso 1 1 calc R . . C56 C 0.2605(4) 0.2953(2) 0.5578(3) 0.0249(12) Uani 1 1 d . . . H56 H 0.2172 0.3017 0.5895 0.030 Uiso 1 1 calc R . . C62 C 0.6109(3) 0.26375(18) 0.6864(3) 0.0195(10) Uani 1 1 d . . . H62 H 0.5891 0.2304 0.6801 0.023 Uiso 1 1 calc R . . C48 C 0.4928(3) 0.2092(2) 1.0794(3) 0.0304(13) Uani 1 1 d . . . H48 H 0.5340 0.2371 1.0926 0.037 Uiso 1 1 calc R . . C54 C 0.0804(4) 0.30484(19) 0.8885(3) 0.0291(12) Uani 1 1 d . . . H54 H 0.0430 0.3190 0.8486 0.035 Uiso 1 1 calc R . . C57 C 0.2227(4) 0.2932(2) 0.4873(3) 0.0248(12) Uani 1 1 d . . . H57 H 0.1544 0.2992 0.4720 0.030 Uiso 1 1 calc R . . C52 C 0.1374(3) 0.30604(18) 1.0114(3) 0.0206(11) Uani 1 1 d . . . H52 H 0.1388 0.3216 1.0545 0.025 Uiso 1 1 calc R . . C53 C 0.0823(4) 0.32761(18) 0.9518(3) 0.0254(12) Uani 1 1 d . . . H53 H 0.0468 0.3575 0.9549 0.030 Uiso 1 1 calc R . . C47 C 0.5110(4) 0.1630(2) 1.1148(3) 0.0356(14) Uani 1 1 d . . . H47 H 0.5644 0.1603 1.1518 0.043 Uiso 1 1 calc R . . C46 C 0.4511(4) 0.1221(2) 1.0955(3) 0.0352(14) Uani 1 1 d . . . H46 H 0.4648 0.0914 1.1187 0.042 Uiso 1 1 calc R . . C60 C 0.4249(4) 0.2767(2) 0.5333(3) 0.0251(12) Uani 1 1 d . . . H60 H 0.4933 0.2708 0.5483 0.030 Uiso 1 1 calc R . . C72 C 0.3246(3) 0.38383(17) 0.6736(3) 0.0178(10) Uani 1 1 d . . . H72 H 0.3457 0.3881 0.6308 0.021 Uiso 1 1 calc R . . C58 C 0.2846(4) 0.2824(2) 0.4396(3) 0.0294(13) Uani 1 1 d . . . H58 H 0.2585 0.2807 0.3922 0.035 Uiso 1 1 calc R . . C69 C 0.2595(3) 0.37163(18) 0.8016(3) 0.0213(11) Uani 1 1 d . . . H69 H 0.2376 0.3675 0.8442 0.026 Uiso 1 1 calc R . . C68 C 0.3083(3) 0.33193(18) 0.7725(3) 0.0188(10) Uani 1 1 d . . . H68 H 0.3179 0.3012 0.7961 0.023 Uiso 1 1 calc R . . C67 C 0.3425(3) 0.33742(16) 0.7093(2) 0.0145(9) Uani 1 1 d . . . C59 C 0.3855(4) 0.2741(2) 0.4629(3) 0.0317(13) Uani 1 1 d . . . H59 H 0.4280 0.2667 0.4309 0.038 Uiso 1 1 calc R . . C65 C 0.6772(4) 0.3626(2) 0.7094(3) 0.0329(14) Uani 1 1 d . . . H65 H 0.6998 0.3956 0.7192 0.039 Uiso 1 1 calc R . . C64 C 0.7472(4) 0.3241(2) 0.7046(3) 0.0308(13) Uani 1 1 d . . . H64 H 0.8155 0.3317 0.7080 0.037 Uiso 1 1 calc R . . C71 C 0.2762(3) 0.42314(18) 0.7014(3) 0.0222(11) Uani 1 1 d . . . H71 H 0.2647 0.4535 0.6772 0.027 Uiso 1 1 calc R . . C70 C 0.2447(3) 0.41731(19) 0.7654(3) 0.0243(12) Uani 1 1 d . . . H70 H 0.2133 0.4441 0.7843 0.029 Uiso 1 1 calc R . . I2 I 0.49019(2) 0.201126(10) 0.841477(15) 0.01374(8) Uani 1 1 d . . . I4 I 0.18099(2) 0.195864(11) 0.712164(16) 0.01484(8) Uani 1 1 d . . . I1 I 0.44107(2) 0.139120(11) 0.627556(15) 0.01390(8) Uani 1 1 d . . . I3 I 0.32935(2) 0.062513(10) 0.808650(16) 0.01539(8) Uani 1 1 d . . . Cu4 Cu 0.37883(4) 0.20670(2) 0.71623(3) 0.01511(13) Uani 1 1 d . . . Cu1 Cu 0.47575(4) 0.11647(2) 0.76375(3) 0.01508(13) Uani 1 1 d . . . Cu2 Cu 0.28418(4) 0.11234(2) 0.68837(3) 0.01590(13) Uani 1 1 d . . . Cu3 Cu 0.30168(4) 0.16281(2) 0.82811(3) 0.01636(13) Uani 1 1 d . . . P1 P 0.61921(8) 0.07042(4) 0.78532(6) 0.0134(2) Uani 1 1 d . . . P4 P 0.40651(8) 0.28449(4) 0.67509(6) 0.0132(2) Uani 1 1 d . . . P3 P 0.24774(8) 0.17600(4) 0.93100(7) 0.0148(2) Uani 1 1 d . . . P2 P 0.17886(8) 0.06615(4) 0.61048(6) 0.0141(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 C25 0.015(2) 0.009(2) 0.013(2) 0.0018(17) 0.0005(18) -0.0023(17) C1 0.017(2) 0.012(2) 0.013(2) -0.0012(18) -0.0043(18) 0.0002(18) C20 0.020(2) 0.017(2) 0.024(3) -0.004(2) 0.001(2) -0.0007(19) C4 0.024(2) 0.016(2) 0.021(3) -0.005(2) -0.004(2) 0.002(2) C28 0.027(3) 0.023(3) 0.020(3) -0.001(2) 0.008(2) 0.004(2) C31 0.024(2) 0.010(2) 0.018(3) -0.0010(19) -0.004(2) -0.0015(19) C13 0.017(2) 0.014(2) 0.016(2) -0.0004(19) -0.0046(19) -0.0037(18) C2 0.017(2) 0.015(2) 0.026(3) 0.000(2) 0.002(2) 0.0000(19) C37 0.019(2) 0.013(2) 0.024(3) 0.008(2) 0.006(2) 0.0066(19) C30 0.017(2) 0.014(2) 0.016(2) 0.0036(19) 0.0009(19) 0.0026(18) C24 0.016(2) 0.013(2) 0.018(2) -0.0010(19) -0.0002(19) 0.0003(18) C8 0.014(2) 0.017(2) 0.023(3) -0.001(2) 0.0010(19) 0.0043(19) C23 0.022(2) 0.014(2) 0.029(3) -0.004(2) 0.005(2) -0.002(2) C3 0.020(2) 0.017(2) 0.025(3) -0.006(2) 0.004(2) 0.004(2) C10 0.018(2) 0.010(2) 0.029(3) -0.002(2) -0.007(2) 0.0041(18) C29 0.026(3) 0.024(3) 0.022(3) 0.003(2) -0.002(2) 0.006(2) C7 0.016(2) 0.008(2) 0.020(2) 0.0020(19) 0.0034(19) 0.0047(18) C33 0.023(3) 0.028(3) 0.030(3) -0.004(2) -0.007(2) 0.010(2) C9 0.026(3) 0.014(2) 0.027(3) 0.007(2) 0.006(2) 0.005(2) C32 0.019(2) 0.020(2) 0.023(3) -0.001(2) -0.001(2) 0.004(2) C27 0.035(3) 0.024(3) 0.016(3) -0.001(2) 0.000(2) -0.006(2) C19 0.011(2) 0.011(2) 0.017(2) -0.0017(18) -0.0010(18) 0.0007(17) C5 0.020(2) 0.015(2) 0.030(3) 0.000(2) 0.000(2) -0.002(2) C26 0.017(2) 0.017(2) 0.017(2) 0.0004(19) 0.0007(19) 0.0005(19) C17 0.022(2) 0.014(2) 0.030(3) 0.003(2) -0.010(2) -0.001(2) C42 0.015(2) 0.029(3) 0.020(3) 0.002(2) -0.0022(19) 0.000(2) C34 0.027(3) 0.028(3) 0.031(3) 0.010(2) -0.005(2) -0.012(2) C22 0.016(2) 0.027(3) 0.024(3) 0.009(2) 0.002(2) 0.001(2) C40 0.018(2) 0.021(3) 0.048(4) 0.005(3) 0.009(2) -0.004(2) C41 0.021(3) 0.022(3) 0.035(3) 0.009(2) -0.006(2) -0.004(2) C35 0.040(3) 0.021(3) 0.027(3) 0.011(2) -0.011(3) -0.017(2) C6 0.021(2) 0.017(2) 0.027(3) -0.002(2) 0.002(2) -0.002(2) C11 0.020(2) 0.018(3) 0.040(3) -0.005(2) -0.003(2) 0.000(2) C16 0.016(2) 0.014(2) 0.023(3) 0.000(2) -0.0012(19) 0.0007(18) C14 0.037(3) 0.028(3) 0.021(3) 0.000(2) 0.002(2) 0.014(2) C15 0.053(4) 0.037(3) 0.019(3) 0.003(3) 0.005(3) 0.017(3) C21 0.015(2) 0.027(3) 0.027(3) -0.002(2) 0.005(2) 0.000(2) C38 0.038(3) 0.015(3) 0.049(4) -0.005(2) 0.020(3) -0.010(2) C39 0.036(3) 0.022(3) 0.054(4) 0.000(3) 0.029(3) -0.006(2) C43 0.012(2) 0.020(2) 0.019(3) 0.001(2) 0.0060(18) 0.0008(18) C50 0.037(3) 0.017(2) 0.021(3) 0.006(2) 0.013(2) 0.010(2) C49 0.023(2) 0.010(2) 0.022(3) 0.0007(19) 0.010(2) 0.0002(19) C44 0.017(2) 0.026(3) 0.028(3) 0.005(2) 0.005(2) -0.003(2) C12 0.013(2) 0.013(2) 0.051(4) 0.004(2) 0.005(2) 0.0035(19) C45 0.024(3) 0.025(3) 0.027(3) 0.004(2) 0.000(2) 0.005(2) C36 0.042(3) 0.013(2) 0.027(3) 0.001(2) -0.015(3) 0.006(2) C51 0.017(2) 0.014(2) 0.027(3) -0.003(2) 0.001(2) -0.0006(19) C18 0.049(3) 0.025(3) 0.018(3) 0.006(2) -0.005(3) -0.002(3) C61 0.012(2) 0.016(2) 0.019(3) -0.0015(19) 0.0019(19) -0.0014(18) C55 0.017(2) 0.007(2) 0.018(2) 0.0014(18) 0.0041(19) 0.0020(17) C66 0.019(2) 0.018(3) 0.043(4) -0.012(2) 0.000(2) -0.003(2) C63 0.012(2) 0.024(3) 0.038(3) -0.009(2) -0.004(2) 0.006(2) C56 0.016(2) 0.038(3) 0.019(3) 0.000(2) -0.001(2) -0.002(2) C62 0.016(2) 0.016(2) 0.025(3) -0.001(2) -0.001(2) 0.0000(19) C48 0.009(2) 0.041(3) 0.040(4) -0.009(3) 0.002(2) -0.008(2) C54 0.040(3) 0.020(3) 0.029(3) 0.006(2) 0.009(3) 0.006(2) C57 0.020(2) 0.035(3) 0.017(3) 0.000(2) -0.004(2) 0.001(2) C52 0.019(2) 0.018(2) 0.025(3) -0.009(2) 0.005(2) -0.0009(19) C53 0.023(2) 0.013(2) 0.042(3) 0.000(2) 0.011(2) 0.001(2) C47 0.024(3) 0.064(4) 0.019(3) 0.005(3) 0.000(2) 0.005(3) C46 0.032(3) 0.045(4) 0.028(3) 0.016(3) 0.002(3) 0.008(3) C60 0.017(2) 0.034(3) 0.023(3) 0.004(2) -0.002(2) -0.001(2) C72 0.021(2) 0.018(2) 0.016(2) 0.0031(19) 0.0077(19) -0.0019(19) C58 0.040(3) 0.027(3) 0.017(3) 0.000(2) -0.009(2) 0.000(2) C69 0.023(2) 0.023(3) 0.019(3) -0.005(2) 0.005(2) -0.006(2) C68 0.016(2) 0.017(2) 0.023(3) 0.001(2) 0.0019(19) -0.0003(19) C67 0.009(2) 0.012(2) 0.021(3) -0.0007(19) -0.0030(18) -0.0011(17) C59 0.037(3) 0.038(3) 0.022(3) 0.000(3) 0.010(2) 0.005(3) C65 0.017(3) 0.019(3) 0.063(4) -0.018(3) 0.009(3) -0.002(2) C64 0.015(2) 0.029(3) 0.046(4) -0.009(3) -0.002(2) -0.003(2) C71 0.023(2) 0.018(2) 0.024(3) 0.002(2) 0.000(2) 0.008(2) C70 0.017(2) 0.020(3) 0.034(3) -0.011(2) 0.000(2) 0.003(2) I2 0.01354(14) 0.01203(14) 0.01407(16) -0.00093(11) -0.00236(11) -0.00074(11) I4 0.01214(14) 0.01319(15) 0.01793(16) -0.00072(12) -0.00121(12) 0.00105(11) I1 0.01459(14) 0.01213(14) 0.01442(15) -0.00022(11) 0.00076(11) -0.00133(11) I3 0.01697(15) 0.00944(14) 0.01961(17) 0.00162(11) 0.00258(12) -0.00072(11) Cu4 0.0155(3) 0.0113(3) 0.0175(3) 0.0017(2) -0.0005(2) 0.0000(2) Cu1 0.0140(3) 0.0121(3) 0.0180(3) 0.0010(2) -0.0007(2) 0.0010(2) Cu2 0.0141(3) 0.0138(3) 0.0186(3) -0.0020(2) -0.0010(2) -0.0017(2) Cu3 0.0175(3) 0.0130(3) 0.0183(3) 0.0009(2) 0.0024(2) 0.0005(2) P1 0.0123(5) 0.0115(5) 0.0155(6) 0.0002(5) -0.0004(5) 0.0006(4) P4 0.0126(5) 0.0101(5) 0.0162(6) -0.0002(5) 0.0000(5) 0.0012(4) P3 0.0161(6) 0.0105(5) 0.0179(6) 0.0020(5) 0.0037(5) 0.0000(5) P2 0.0137(5) 0.0118(5) 0.0157(6) -0.0008(5) -0.0011(5) -0.0021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C25 C30 1.399(6) . ? C25 C26 1.408(6) . ? C25 P2 1.808(5) . ? C1 C2 1.395(7) . ? C1 C6 1.399(6) . ? C1 P1 1.834(5) . ? C20 C21 1.388(7) . ? C20 C19 1.392(7) . ? C20 H20 0.9300 . ? C4 C5 1.371(7) . ? C4 C3 1.374(7) . ? C4 H4 0.9300 . ? C28 C29 1.379(7) . ? C28 C27 1.387(7) . ? C28 H28 0.9300 . ? C31 C34 1.391(7) . ? C31 C32 1.402(6) . ? C31 P2 1.829(5) . ? C13 C14 1.389(7) . ? C13 C16 1.405(6) . ? C13 P1 1.824(5) . ? C2 C3 1.394(6) . ? C2 H2 0.9300 . ? C37 C38 1.384(8) . ? C37 C42 1.404(7) . ? C37 P3 1.838(5) . ? C30 C29 1.400(7) . ? C30 H30 0.9300 . ? C24 C23 1.386(7) . ? C24 C19 1.402(6) . ? C24 H24 0.9300 . ? C8 C9 1.393(7) . ? C8 C7 1.400(7) . ? C8 H8 0.9300 . ? C23 C22 1.383(7) . ? C23 H23 0.9300 . ? C3 H3 0.9300 . ? C10 C7 1.396(6) . ? C10 C11 1.388(7) . ? C10 H10 0.9300 . ? C29 H29 0.9300 . ? C7 P1 1.831(5) . ? C33 C36 1.370(8) . ? C33 C32 1.381(7) . ? C33 H33 0.9300 . ? C9 C12 1.386(7) . ? C9 H9 0.9300 . ? C32 H32 0.9300 . ? C27 C26 1.378(7) . ? C27 H27 0.9300 . ? C19 P2 1.824(5) . ? C5 C6 1.398(6) . ? C5 H5 0.9300 . ? C26 H26 0.9300 . ? C17 C18 1.376(8) . ? C17 C16 1.390(7) . ? C17 H17 0.9300 . ? C42 C41 1.393(7) . ? C42 H42 0.9300 . ? C34 C35 1.382(7) . ? C34 H34 0.9300 . ? C22 C21 1.386(7) . ? C22 H22 0.9300 . ? C40 C41 1.360(8) . ? C40 C39 1.370(8) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C35 C36 1.381(8) . ? C35 H35 0.9300 . ? C6 H6 0.9300 . ? C11 C12 1.382(8) . ? C11 H11 0.9300 . ? C16 H16 0.9300 . ? C14 C15 1.403(7) . ? C14 H14 0.9300 . ? C15 C18 1.380(8) . ? C15 H15 0.9300 . ? C21 H21 0.9300 . ? C38 C39 1.387(7) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C43 C45 1.395(7) . ? C43 C44 1.413(7) . ? C43 P3 1.820(5) . ? C50 C54 1.385(7) . ? C50 C49 1.392(6) . ? C50 H50 0.9300 . ? C49 C51 1.389(7) . ? C49 P3 1.840(5) . ? C44 C48 1.370(7) . ? C44 H44 0.9300 . ? C12 H12 0.9300 . ? C45 C46 1.390(7) . ? C45 H45 0.9300 . ? C36 H36 0.9300 . ? C51 C52 1.394(6) . ? C51 H51 0.9300 . ? C18 H18 0.9300 . ? C61 C66 1.394(6) . ? C61 C62 1.398(6) . ? C61 P4 1.838(4) . ? C55 C60 1.388(7) . ? C55 C56 1.388(6) . ? C55 P4 1.814(5) . ? C66 C65 1.390(7) . ? C66 H66 0.9300 . ? C63 C64 1.373(7) . ? C63 C62 1.404(6) . ? C63 H63 0.9300 . ? C56 C57 1.381(7) . ? C56 H56 0.9300 . ? C62 H62 0.9300 . ? C48 C47 1.403(8) . ? C48 H48 0.9300 . ? C54 C53 1.364(8) . ? C54 H54 0.9300 . ? C57 C58 1.374(8) . ? C57 H57 0.9300 . ? C52 C53 1.390(7) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C47 C46 1.363(8) . ? C47 H47 0.9300 . ? C46 H46 0.9300 . ? C60 C59 1.385(7) . ? C60 H60 0.9300 . ? C72 C71 1.381(7) . ? C72 C67 1.409(6) . ? C72 H72 0.9300 . ? C58 C59 1.373(7) . ? C58 H58 0.9300 . ? C69 C70 1.394(7) . ? C69 C68 1.404(7) . ? C69 H69 0.9300 . ? C68 C67 1.387(7) . ? C68 H68 0.9300 . ? C67 P4 1.823(5) . ? C59 H59 0.9300 . ? C65 C64 1.398(7) . ? C65 H65 0.9300 . ? C64 H64 0.9300 . ? C71 C70 1.386(7) . ? C71 H71 0.9300 . ? C70 H70 0.9300 . ? I2 Cu4 2.6404(7) . ? I2 Cu1 2.6866(6) . ? I2 Cu3 2.6976(6) . ? I4 Cu4 2.6593(6) . ? I4 Cu2 2.6849(6) . ? I4 Cu3 2.6929(7) . ? I1 Cu2 2.6749(7) . ? I1 Cu1 2.6770(7) . ? I1 Cu4 2.7066(7) . ? I3 Cu2 2.6626(7) . ? I3 Cu1 2.6872(6) . ? I3 Cu3 2.7096(7) . ? Cu4 P4 2.2573(13) . ? Cu4 Cu1 2.7970(8) . ? Cu4 Cu2 2.8084(8) . ? Cu4 Cu3 2.8081(9) . ? Cu1 P1 2.2574(12) . ? Cu1 Cu2 2.7426(8) . ? Cu2 P2 2.2513(12) . ? Cu2 Cu3 2.9983(8) . ? Cu3 P3 2.2626(14) . ? 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 C30 C25 C26 118.2(4) . . ? C30 C25 P2 119.0(3) . . ? C26 C25 P2 122.8(3) . . ? C2 C1 C6 118.1(4) . . ? C2 C1 P1 124.8(3) . . ? C6 C1 P1 117.0(4) . . ? C21 C20 C19 121.2(5) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C5 C4 C3 119.5(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C29 C28 C27 120.5(5) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C34 C31 C32 118.3(4) . . ? C34 C31 P2 118.4(4) . . ? C32 C31 P2 123.2(4) . . ? C14 C13 C16 119.6(4) . . ? C14 C13 P1 119.7(4) . . ? C16 C13 P1 120.7(4) . . ? C3 C2 C1 121.1(4) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C38 C37 C42 119.0(5) . . ? C38 C37 P3 122.1(4) . . ? C42 C37 P3 118.8(4) . . ? C29 C30 C25 120.8(4) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? C23 C24 C19 119.9(4) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C9 C8 C7 120.8(4) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C22 C23 C24 120.3(5) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C4 C3 C2 120.2(5) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C7 C10 C11 120.1(5) . . ? C7 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C28 C29 C30 119.6(4) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C10 C7 C8 118.5(4) . . ? C10 C7 P1 122.4(4) . . ? C8 C7 P1 118.8(3) . . ? C36 C33 C32 120.5(5) . . ? C36 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C12 C9 C8 119.9(5) . . ? C12 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C33 C32 C31 120.1(5) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C26 C27 C28 120.3(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C20 C19 C24 118.8(4) . . ? C20 C19 P2 117.8(3) . . ? C24 C19 P2 123.3(4) . . ? C4 C5 C6 121.4(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C27 C26 C25 120.7(4) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C18 C17 C16 119.6(5) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C41 C42 C37 119.2(5) . . ? C41 C42 H42 120.4 . . ? C37 C42 H42 120.4 . . ? C35 C34 C31 121.0(5) . . ? C35 C34 H34 119.5 . . ? C31 C34 H34 119.5 . . ? C23 C22 C21 120.7(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C41 C40 C39 120.6(5) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C42 120.8(5) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C34 C35 C36 119.6(5) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C5 C6 C1 119.7(5) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C12 C11 C10 121.0(5) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C17 C16 C13 120.3(5) . . ? C17 C16 H16 119.8 . . ? C13 C16 H16 119.8 . . ? C13 C14 C15 119.4(5) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C18 C15 C14 120.2(6) . . ? C18 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C22 C21 C20 119.1(5) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C37 C38 C39 120.6(5) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C40 C39 C38 119.9(6) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C45 C43 C44 118.5(4) . . ? C45 C43 P3 120.8(4) . . ? C44 C43 P3 120.5(4) . . ? C54 C50 C49 121.4(5) . . ? C54 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? C51 C49 C50 118.1(4) . . ? C51 C49 P3 124.2(4) . . ? C50 C49 P3 117.5(4) . . ? C48 C44 C43 120.7(5) . . ? C48 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C11 C12 C9 119.5(5) . . ? C11 C12 H12 120.2 . . ? C9 C12 H12 120.2 . . ? C46 C45 C43 120.2(5) . . ? C46 C45 H45 119.9 . . ? C43 C45 H45 119.9 . . ? C33 C36 C35 120.3(5) . . ? C33 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C49 C51 C52 120.4(5) . . ? C49 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C17 C18 C15 120.9(5) . . ? C17 C18 H18 119.5 . . ? C15 C18 H18 119.5 . . ? C66 C61 C62 119.3(4) . . ? C66 C61 P4 123.5(4) . . ? C62 C61 P4 117.1(3) . . ? C60 C55 C56 118.4(5) . . ? C60 C55 P4 122.4(3) . . ? C56 C55 P4 118.7(4) . . ? C61 C66 C65 119.8(5) . . ? C61 C66 H66 120.1 . . ? C65 C66 H66 120.1 . . ? C64 C63 C62 120.3(5) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C57 C56 C55 120.4(5) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C61 C62 C63 120.1(4) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C44 C48 C47 119.5(5) . . ? C44 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C53 C54 C50 120.0(5) . . ? C53 C54 H54 120.0 . . ? C50 C54 H54 120.0 . . ? C56 C57 C58 120.9(5) . . ? C56 C57 H57 119.5 . . ? C58 C57 H57 119.5 . . ? C51 C52 C53 120.1(5) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 119.9(5) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C46 C47 C48 120.5(5) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C47 C46 C45 120.5(5) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C59 C60 C55 120.4(5) . . ? C59 C60 H60 119.8 . . ? C55 C60 H60 119.8 . . ? C71 C72 C67 121.0(5) . . ? C71 C72 H72 119.5 . . ? C67 C72 H72 119.5 . . ? C59 C58 C57 119.0(5) . . ? C59 C58 H58 120.5 . . ? C57 C58 H58 120.5 . . ? C70 C69 C68 118.7(5) . . ? C70 C69 H69 120.7 . . ? C68 C69 H69 120.7 . . ? C67 C68 C69 121.6(4) . . ? C67 C68 H68 119.2 . . ? C69 C68 H68 119.2 . . ? C68 C67 C72 118.1(4) . . ? C68 C67 P4 119.2(3) . . ? C72 C67 P4 122.7(4) . . ? C58 C59 C60 120.8(5) . . ? C58 C59 H59 119.6 . . ? C60 C59 H59 119.6 . . ? C66 C65 C64 120.7(5) . . ? C66 C65 H65 119.6 . . ? C64 C65 H65 119.6 . . ? C63 C64 C65 119.5(5) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C72 C71 C70 120.0(5) . . ? C72 C71 H71 120.0 . . ? C70 C71 H71 120.0 . . ? C71 C70 C69 120.6(5) . . ? C71 C70 H70 119.7 . . ? C69 C70 H70 119.7 . . ? Cu4 I2 Cu1 63.337(18) . . ? Cu4 I2 Cu3 63.469(19) . . ? Cu1 I2 Cu3 69.794(19) . . ? Cu4 I4 Cu2 63.402(18) . . ? Cu4 I4 Cu3 63.288(19) . . ? Cu2 I4 Cu3 67.771(19) . . ? Cu2 I1 Cu1 61.655(19) . . ? Cu2 I1 Cu4 62.911(18) . . ? Cu1 I1 Cu4 62.599(18) . . ? Cu2 I3 Cu1 61.680(18) . . ? Cu2 I3 Cu3 67.844(19) . . ? Cu1 I3 Cu3 69.608(19) . . ? P4 Cu4 I2 106.01(4) . . ? P4 Cu4 I4 108.03(4) . . ? I2 Cu4 I4 115.57(2) . . ? P4 Cu4 I1 106.76(4) . . ? I2 Cu4 I1 111.25(2) . . ? I4 Cu4 I1 108.79(2) . . ? P4 Cu4 Cu1 142.87(4) . . ? I2 Cu4 Cu1 59.137(17) . . ? I4 Cu4 Cu1 109.02(2) . . ? I1 Cu4 Cu1 58.182(18) . . ? P4 Cu4 Cu2 146.60(4) . . ? I2 Cu4 Cu2 107.29(2) . . ? I4 Cu4 Cu2 58.742(17) . . ? I1 Cu4 Cu2 57.992(18) . . ? Cu1 Cu4 Cu2 58.59(2) . . ? P4 Cu4 Cu3 138.86(4) . . ? I2 Cu4 Cu3 59.258(18) . . ? I4 Cu4 Cu3 58.940(18) . . ? I1 Cu4 Cu3 114.38(2) . . ? Cu1 Cu4 Cu3 66.67(2) . . ? Cu2 Cu4 Cu3 64.53(2) . . ? P1 Cu1 I1 107.89(4) . . ? P1 Cu1 I2 111.34(4) . . ? I1 Cu1 I2 110.74(2) . . ? P1 Cu1 I3 107.54(4) . . ? I1 Cu1 I3 114.99(2) . . ? I2 Cu1 I3 104.32(2) . . ? P1 Cu1 Cu2 140.66(4) . . ? I1 Cu1 Cu2 59.134(19) . . ? I2 Cu1 Cu2 107.89(2) . . ? I3 Cu1 Cu2 58.720(18) . . ? P1 Cu1 Cu4 148.87(4) . . ? I1 Cu1 Cu4 59.219(18) . . ? I2 Cu1 Cu4 57.526(18) . . ? I3 Cu1 Cu4 103.51(2) . . ? Cu2 Cu1 Cu4 60.914(19) . . ? P2 Cu2 I3 110.39(4) . . ? P2 Cu2 I1 107.40(4) . . ? I3 Cu2 I1 115.89(2) . . ? P2 Cu2 I4 106.04(4) . . ? I3 Cu2 I4 107.69(2) . . ? I1 Cu2 I4 108.98(2) . . ? P2 Cu2 Cu1 144.03(4) . . ? I3 Cu2 Cu1 59.600(18) . . ? I1 Cu2 Cu1 59.211(18) . . ? I4 Cu2 Cu1 109.90(2) . . ? P2 Cu2 Cu4 145.48(4) . . ? I3 Cu2 Cu4 103.84(2) . . ? I1 Cu2 Cu4 59.098(18) . . ? I4 Cu2 Cu4 57.855(18) . . ? Cu1 Cu2 Cu4 60.500(19) . . ? P2 Cu2 Cu3 142.73(4) . . ? I3 Cu2 Cu3 56.822(18) . . ? I1 Cu2 Cu3 109.45(2) . . ? I4 Cu2 Cu3 56.243(17) . . ? Cu1 Cu2 Cu3 64.72(2) . . ? Cu4 Cu2 Cu3 57.73(2) . . ? P3 Cu3 I4 116.93(4) . . ? P3 Cu3 I2 106.83(4) . . ? I4 Cu3 I2 112.57(2) . . ? P3 Cu3 I3 110.18(4) . . ? I4 Cu3 I3 106.11(2) . . ? I2 Cu3 I3 103.41(2) . . ? P3 Cu3 Cu4 146.43(4) . . ? I4 Cu3 Cu4 57.772(18) . . ? I2 Cu3 Cu4 57.273(18) . . ? I3 Cu3 Cu4 102.63(2) . . ? P3 Cu3 Cu2 151.60(4) . . ? I4 Cu3 Cu2 55.987(17) . . ? I2 Cu3 Cu2 100.69(2) . . ? I3 Cu3 Cu2 55.334(17) . . ? Cu4 Cu3 Cu2 57.74(2) . . ? C13 P1 C1 101.5(2) . . ? C13 P1 C7 104.3(2) . . ? C1 P1 C7 105.4(2) . . ? C13 P1 Cu1 116.24(16) . . ? C1 P1 Cu1 115.14(14) . . ? C7 P1 Cu1 112.86(14) . . ? C55 P4 C67 103.5(2) . . ? C55 P4 C61 105.4(2) . . ? C67 P4 C61 105.2(2) . . ? C55 P4 Cu4 110.70(14) . . ? C67 P4 Cu4 116.97(16) . . ? C61 P4 Cu4 113.92(15) . . ? C43 P3 C49 103.7(2) . . ? C43 P3 C37 103.7(2) . . ? C49 P3 C37 101.5(2) . . ? C43 P3 Cu3 112.90(15) . . ? C49 P3 Cu3 116.78(16) . . ? C37 P3 Cu3 116.52(17) . . ? C25 P2 C19 105.6(2) . . ? C25 P2 C31 103.2(2) . . ? C19 P2 C31 103.8(2) . . ? C25 P2 Cu2 115.40(14) . . ? C19 P2 Cu2 114.26(15) . . ? C31 P2 Cu2 113.39(15) . . ? _diffrn_measured_fraction_theta_max 0.849 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.259 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.204 # Attachment '- 1b_90k.cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 838120' #TrackingRef '- 1b_90k.cif' _cell_special_details ? #Added by publCIF _symmetry_space_group_name_hall ? #Added by publCIF _audit_update_record ; 2011-06-28 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _chemical_formula_weight 1810.84 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I -4 3 d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z+1/2' '-x, -y+1/2, z' '-x, y+1/2, -z+1/2' 'y+1/4, -x+3/4, -z+1/4' '-y+1/4, -x+3/4, z+3/4' '-y+3/4, x+3/4, -z+1/4' 'y+3/4, x+3/4, z+3/4' 'y, z, x' '-y, -z+1/2, x' 'y, -z, -x+1/2' '-y, z+1/2, -x+1/2' 'z+1/4, -y+3/4, -x+1/4' 'z+1/4, y+1/4, x+1/4' '-z+3/4, y+3/4, -x+1/4' '-z+3/4, -y+1/4, x+1/4' 'z, x, y' '-z+1/2, x, -y' '-z, -x+1/2, y' 'z+1/2, -x+1/2, -y' 'x+3/4, z+3/4, y+3/4' 'x+3/4, -z+1/4, -y+3/4' '-x+3/4, z+3/4, -y+1/4' '-x+1/4, -z+3/4, y+3/4' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1' 'y+3/4, -x+5/4, -z+3/4' '-y+3/4, -x+5/4, z+5/4' '-y+5/4, x+5/4, -z+3/4' 'y+5/4, x+5/4, z+5/4' 'y+1/2, z+1/2, x+1/2' '-y+1/2, -z+1, x+1/2' 'y+1/2, -z+1/2, -x+1' '-y+1/2, z+1, -x+1' 'z+3/4, -y+5/4, -x+3/4' 'z+3/4, y+3/4, x+3/4' '-z+5/4, y+5/4, -x+3/4' '-z+5/4, -y+3/4, x+3/4' 'z+1/2, x+1/2, y+1/2' '-z+1, x+1/2, -y+1/2' '-z+1/2, -x+1, y+1/2' 'z+1, -x+1, -y+1/2' 'x+5/4, z+5/4, y+5/4' 'x+5/4, -z+3/4, -y+5/4' '-x+5/4, z+5/4, -y+3/4' '-x+3/4, -z+5/4, y+5/4' _cell_length_a 29.7864(3) _cell_length_b 29.7864(3) _cell_length_c 29.7864(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26427.4(5) _cell_formula_units_Z 16 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 5147 _cell_measurement_theta_min 2.5534 _cell_measurement_theta_max 29.0959 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14080 _exptl_absorpt_coefficient_mu 3.278 _exptl_absorpt_correction_T_min 0.98614 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 90(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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13317 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 29.01 _reflns_number_total 4275 _reflns_number_gt 3850 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 4275 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 C2 C 0.49555(18) 0.53371(17) 0.17472(17) 0.0187(12) Uani 1 1 d . . . H2 H 0.4649 0.5352 0.1688 0.022 Uiso 1 1 calc R . . C7 C 0.44091(18) 0.44235(17) 0.15659(16) 0.0134(11) Uani 1 1 d . . . C15 C 0.56032(19) 0.3357(2) 0.1102(2) 0.0276(15) Uani 1 1 d . . . H15 H 0.5689 0.3179 0.0861 0.033 Uiso 1 1 calc R . . C3 C 0.5160(2) 0.56781(18) 0.19841(18) 0.0224(13) Uani 1 1 d . . . H3 H 0.4990 0.5915 0.2095 0.027 Uiso 1 1 calc R . . C12 C 0.43863(18) 0.4453(2) 0.20335(18) 0.0221(13) Uani 1 1 d . . . H12 H 0.4629 0.4569 0.2193 0.026 Uiso 1 1 calc R . . C8 C 0.40360(18) 0.42558(18) 0.1341(2) 0.0206(13) Uani 1 1 d . . . H8 H 0.4039 0.4237 0.1030 0.025 Uiso 1 1 calc R . . C13 C 0.52419(18) 0.40287(18) 0.13773(18) 0.0176(12) Uani 1 1 d . . . C4 C 0.5620(2) 0.56666(19) 0.20573(18) 0.0245(14) Uani 1 1 d . . . H4 H 0.5761 0.5897 0.2214 0.029 Uiso 1 1 calc R . . C1 C 0.52013(17) 0.49705(17) 0.15954(17) 0.0139(11) Uani 1 1 d . . . C9 C 0.3661(2) 0.41162(19) 0.1576(2) 0.0262(14) Uani 1 1 d . . . H9 H 0.3415 0.4003 0.1421 0.031 Uiso 1 1 calc R . . C14 C 0.53865(18) 0.37626(18) 0.10290(19) 0.0191(12) Uani 1 1 d . . . H14 H 0.5337 0.3857 0.0736 0.023 Uiso 1 1 calc R . . C5 C 0.5864(2) 0.53097(19) 0.1894(2) 0.0278(14) Uani 1 1 d . . . H5 H 0.6173 0.5302 0.1939 0.033 Uiso 1 1 calc R . . C19 C 0.64124(17) 0.42989(17) -0.07601(17) 0.0143(11) Uani 1 1 d . . . C17 C 0.5557(2) 0.3488(2) 0.1892(2) 0.044(2) Uani 1 1 d . . . H17 H 0.5613 0.3400 0.2186 0.053 Uiso 1 1 calc R . . C16 C 0.5691(2) 0.32205(19) 0.1539(2) 0.0299(16) Uani 1 1 d . . . H16 H 0.5840 0.2951 0.1593 0.036 Uiso 1 1 calc R . . C11 C 0.4014(2) 0.4315(2) 0.2259(2) 0.0298(16) Uani 1 1 d . . . H11 H 0.4006 0.4337 0.2570 0.036 Uiso 1 1 calc R . . C10 C 0.36485(19) 0.41437(19) 0.2036(2) 0.0257(14) Uani 1 1 d . . . H10 H 0.3397 0.4048 0.2193 0.031 Uiso 1 1 calc R . . C18 C 0.5337(2) 0.3891(2) 0.1807(2) 0.0398(19) Uani 1 1 d . . . H18 H 0.5253 0.4072 0.2048 0.048 Uiso 1 1 calc R . . C24 C 0.67395(18) 0.39725(18) -0.08414(17) 0.0164(12) Uani 1 1 d . . . H24 H 0.6655 0.3689 -0.0940 0.020 Uiso 1 1 calc R . . C23 C 0.71910(18) 0.40702(18) -0.07758(18) 0.0174(12) Uani 1 1 d . . . H23 H 0.7406 0.3850 -0.0827 0.021 Uiso 1 1 calc R . . C22 C 0.73200(18) 0.4488(2) -0.06368(18) 0.0236(13) Uani 1 1 d . . . H22 H 0.7622 0.4549 -0.0588 0.028 Uiso 1 1 calc R . . C21 C 0.70020(18) 0.48212(19) -0.05677(19) 0.0237(13) Uani 1 1 d . . . H21 H 0.7091 0.5107 -0.0479 0.028 Uiso 1 1 calc R . . C6 C 0.56585(17) 0.49620(19) 0.16640(18) 0.0200(13) Uani 1 1 d . . . H6 H 0.5829 0.4723 0.1556 0.024 Uiso 1 1 calc R . . C20 C 0.65462(18) 0.47233(18) -0.06322(18) 0.0185(13) Uani 1 1 d . . . H20 H 0.6332 0.4946 -0.0588 0.022 Uiso 1 1 calc R . . I1 I 0.579120(11) 0.491348(11) 0.038088(11) 0.01345(8) Uani 1 1 d . . . I2 I 0.444893(11) 0.555107(11) 0.055107(11) 0.01489(13) Uani 1 3 d S . . Cu2 Cu 0.53714(2) 0.46286(2) -0.03714(2) 0.0163(2) Uani 1 3 d S . . Cu1 Cu 0.48834(2) 0.47653(2) 0.05395(2) 0.01669(15) Uani 1 1 d . . . P1 P 0.49234(5) 0.45383(5) 0.12588(4) 0.0130(3) Uani 1 1 d . . . P2 P 0.58113(4) 0.41887(4) -0.08113(4) 0.0124(5) Uani 1 3 d S . . 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 C2 0.020(3) 0.016(3) 0.020(3) 0.003(3) -0.002(3) 0.005(3) C7 0.014(2) 0.012(2) 0.014(2) 0.001(2) 0.003(2) 0.001(2) C15 0.021(3) 0.025(3) 0.037(4) -0.018(3) -0.008(3) 0.007(3) C3 0.035(3) 0.016(3) 0.016(3) 0.001(3) -0.001(3) 0.000(3) C12 0.018(3) 0.030(3) 0.018(3) -0.003(3) 0.005(3) -0.001(3) C8 0.018(3) 0.017(3) 0.027(3) -0.001(3) -0.003(3) 0.002(3) C13 0.022(3) 0.015(3) 0.016(3) 0.005(2) 0.000(3) -0.001(3) C4 0.039(4) 0.019(3) 0.015(3) -0.002(3) -0.011(3) -0.008(3) C1 0.016(2) 0.015(3) 0.010(2) 0.006(2) -0.001(2) -0.003(3) C9 0.016(3) 0.023(3) 0.040(4) 0.010(3) -0.006(3) -0.001(3) C14 0.016(3) 0.020(3) 0.022(3) -0.003(3) -0.007(3) 0.001(3) C5 0.029(3) 0.030(3) 0.024(3) -0.002(3) -0.003(3) -0.002(3) C19 0.016(3) 0.016(3) 0.011(2) 0.001(2) 0.004(2) -0.003(2) C17 0.057(4) 0.041(4) 0.034(4) 0.023(4) 0.021(4) 0.035(4) C16 0.024(3) 0.015(3) 0.051(4) 0.009(3) 0.002(3) 0.007(3) C11 0.031(3) 0.036(4) 0.023(3) 0.008(3) 0.005(3) 0.000(3) C10 0.016(3) 0.021(3) 0.040(4) 0.017(3) 0.014(3) 0.001(3) C18 0.063(5) 0.035(4) 0.021(3) 0.005(3) 0.013(4) 0.033(4) C24 0.021(3) 0.012(3) 0.015(3) 0.000(2) 0.000(3) 0.000(3) C23 0.015(3) 0.016(3) 0.022(3) 0.008(3) 0.000(3) 0.001(2) C22 0.013(3) 0.035(3) 0.023(3) 0.008(3) 0.003(3) -0.002(3) C21 0.023(3) 0.021(3) 0.028(3) -0.009(3) 0.004(3) -0.006(3) C6 0.019(3) 0.021(3) 0.020(3) 0.000(3) -0.006(3) 0.001(3) C20 0.019(3) 0.017(3) 0.020(3) -0.001(3) 0.004(3) 0.002(3) I1 0.01264(15) 0.01401(16) 0.01369(16) 0.00003(15) -0.00079(16) 0.00080(14) I2 0.01489(13) 0.01489(13) 0.01489(13) -0.00177(15) 0.00177(15) 0.00177(15) Cu2 0.0163(2) 0.0163(2) 0.0163(2) -0.0017(3) 0.0017(3) 0.0017(3) Cu1 0.0216(4) 0.0165(3) 0.0120(3) 0.0009(3) -0.0012(3) -0.0008(3) P1 0.0151(7) 0.0124(6) 0.0116(6) 0.0000(6) 0.0001(6) 0.0018(6) P2 0.0124(5) 0.0124(5) 0.0124(5) -0.0016(6) 0.0016(6) 0.0016(6) _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 C2 C3 1.378(7) . ? C2 C1 1.390(7) . ? C2 H2 0.9300 . ? C7 C8 1.390(7) . ? C7 C12 1.397(7) . ? C7 P1 1.817(5) . ? C15 C14 1.386(8) . ? C15 C16 1.388(8) . ? C15 H15 0.9300 . ? C3 C4 1.387(8) . ? C3 H3 0.9300 . ? C12 C11 1.360(8) . ? C12 H12 0.9300 . ? C8 C9 1.382(8) . ? C8 H8 0.9300 . ? C13 C14 1.375(7) . ? C13 C18 1.375(8) . ? C13 P1 1.824(5) . ? C4 C5 1.377(8) . ? C4 H4 0.9300 . ? C1 C6 1.377(7) . ? C1 P1 1.830(5) . ? C9 C10 1.371(8) . ? C9 H9 0.9300 . ? C14 H14 0.9300 . ? C5 C6 1.383(7) . ? C5 H5 0.9300 . ? C19 C20 1.379(7) . ? C19 C24 1.398(7) . ? C19 P2 1.827(5) . ? C17 C16 1.380(8) . ? C17 C18 1.388(8) . ? C17 H17 0.9300 . ? C16 H16 0.9300 . ? C11 C10 1.373(8) . ? C11 H11 0.9300 . ? C10 H10 0.9300 . ? C18 H18 0.9300 . ? C24 C23 1.390(7) . ? C24 H24 0.9300 . ? C23 C22 1.366(8) . ? C23 H23 0.9300 . ? C22 C21 1.387(8) . ? C22 H22 0.9300 . ? C21 C20 1.402(7) . ? C21 H21 0.9300 . ? C6 H6 0.9300 . ? C20 H20 0.9300 . ? I1 Cu1 2.6161(7) 12_655 ? I1 Cu2 2.7027(6) . ? I1 Cu1 2.7803(7) . ? I2 Cu1 2.6747(8) . ? I2 Cu1 2.6748(8) 43_554 ? I2 Cu1 2.6748(8) 12_655 ? Cu2 P2 2.270(3) . ? Cu2 I1 2.7025(6) 43_554 ? Cu2 I1 2.7026(6) 12_655 ? Cu1 P1 2.2500(14) . ? Cu1 I1 2.6160(7) 43_554 ? Cu1 Cu1 2.8282(11) 43_554 ? Cu1 Cu1 2.8283(11) 12_655 ? P2 C19 1.827(5) 43_554 ? P2 C19 1.827(5) 12_655 ? 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 C3 C2 C1 120.9(5) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C8 C7 C12 117.6(5) . . ? C8 C7 P1 120.0(4) . . ? C12 C7 P1 122.1(4) . . ? C14 C15 C16 119.4(6) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C2 C3 C4 119.9(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C11 C12 C7 120.8(5) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? C9 C8 C7 120.7(5) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C14 C13 C18 117.8(5) . . ? C14 C13 P1 119.8(4) . . ? C18 C13 P1 122.4(4) . . ? C5 C4 C3 119.0(5) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C1 C2 119.1(5) . . ? C6 C1 P1 121.1(4) . . ? C2 C1 P1 119.5(4) . . ? C10 C9 C8 120.6(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C13 C14 C15 122.0(6) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C20 C19 C24 118.9(5) . . ? C20 C19 P2 118.1(4) . . ? C24 C19 P2 123.0(4) . . ? C16 C17 C18 119.9(6) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C16 C15 119.3(5) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C12 C11 C10 121.4(6) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C9 C10 C11 118.9(5) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C13 C18 C17 121.6(6) . . ? C13 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C23 C24 C19 120.3(5) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C22 C23 C24 120.4(5) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C22 C21 120.3(5) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C21 C20 119.5(5) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C1 C6 C5 119.8(5) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C19 C20 C21 120.5(5) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? Cu1 I1 Cu2 71.40(3) 12_655 . ? Cu1 I1 Cu1 63.13(3) 12_655 . ? Cu2 I1 Cu1 68.96(2) . . ? Cu1 I2 Cu1 63.83(2) . 43_554 ? Cu1 I2 Cu1 63.84(2) . 12_655 ? Cu1 I2 Cu1 63.83(2) 43_554 12_655 ? P2 Cu2 I1 113.13(2) . 43_554 ? P2 Cu2 I1 113.13(2) . 12_655 ? I1 Cu2 I1 105.58(3) 43_554 12_655 ? P2 Cu2 I1 113.13(2) . . ? I1 Cu2 I1 105.58(3) 43_554 . ? I1 Cu2 I1 105.58(3) 12_655 . ? P1 Cu1 I1 120.28(4) . 43_554 ? P1 Cu1 I2 106.04(4) . . ? I1 Cu1 I2 114.71(3) 43_554 . ? P1 Cu1 I1 99.09(4) . . ? I1 Cu1 I1 105.79(3) 43_554 . ? I2 Cu1 I1 109.50(2) . . ? P1 Cu1 Cu1 155.67(5) . 43_554 ? I1 Cu1 Cu1 61.27(2) 43_554 43_554 ? I2 Cu1 Cu1 58.084(12) . 43_554 ? I1 Cu1 Cu1 103.64(2) . 43_554 ? P1 Cu1 Cu1 130.51(5) . 12_655 ? I1 Cu1 Cu1 108.09(2) 43_554 12_655 ? I2 Cu1 Cu1 58.082(12) . 12_655 ? I1 Cu1 Cu1 55.60(2) . 12_655 ? Cu1 Cu1 Cu1 60.0 43_554 12_655 ? C7 P1 C13 100.6(2) . . ? C7 P1 C1 103.8(2) . . ? C13 P1 C1 104.1(2) . . ? C7 P1 Cu1 119.44(17) . . ? C13 P1 Cu1 117.50(18) . . ? C1 P1 Cu1 109.53(17) . . ? C19 P2 C19 104.1(2) . 43_554 ? C19 P2 C19 104.1(2) . 12_655 ? C19 P2 C19 104.1(2) 43_554 12_655 ? C19 P2 Cu2 114.45(17) . . ? C19 P2 Cu2 114.45(17) 43_554 . ? C19 P2 Cu2 114.45(17) 12_655 . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.556 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.095 # Attachment '- 1b_RT.cif' data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 838121' #TrackingRef '- 1b_RT.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _chemical_formula_weight 1810.84 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I -4 3 d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z+1/2' '-x, -y+1/2, z' '-x, y+1/2, -z+1/2' 'y+1/4, -x+3/4, -z+1/4' '-y+1/4, -x+3/4, z+3/4' '-y+3/4, x+3/4, -z+1/4' 'y+3/4, x+3/4, z+3/4' 'y, z, x' '-y, -z+1/2, x' 'y, -z, -x+1/2' '-y, z+1/2, -x+1/2' 'z+1/4, -y+3/4, -x+1/4' 'z+1/4, y+1/4, x+1/4' '-z+3/4, y+3/4, -x+1/4' '-z+3/4, -y+1/4, x+1/4' 'z, x, y' '-z+1/2, x, -y' '-z, -x+1/2, y' 'z+1/2, -x+1/2, -y' 'x+3/4, z+3/4, y+3/4' 'x+3/4, -z+1/4, -y+3/4' '-x+3/4, z+3/4, -y+1/4' '-x+1/4, -z+3/4, y+3/4' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1' 'y+3/4, -x+5/4, -z+3/4' '-y+3/4, -x+5/4, z+5/4' '-y+5/4, x+5/4, -z+3/4' 'y+5/4, x+5/4, z+5/4' 'y+1/2, z+1/2, x+1/2' '-y+1/2, -z+1, x+1/2' 'y+1/2, -z+1/2, -x+1' '-y+1/2, z+1, -x+1' 'z+3/4, -y+5/4, -x+3/4' 'z+3/4, y+3/4, x+3/4' '-z+5/4, y+5/4, -x+3/4' '-z+5/4, -y+3/4, x+3/4' 'z+1/2, x+1/2, y+1/2' '-z+1, x+1/2, -y+1/2' '-z+1/2, -x+1, y+1/2' 'z+1, -x+1, -y+1/2' 'x+5/4, z+5/4, y+5/4' 'x+5/4, -z+3/4, -y+5/4' '-x+5/4, z+5/4, -y+3/4' '-x+3/4, -z+5/4, y+5/4' _cell_length_a 30.0503(6) _cell_length_b 30.0503(6) _cell_length_c 30.0503(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 27136.0(9) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3696 _cell_measurement_theta_min 2.8701 _cell_measurement_theta_max 29.1739 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14080 _exptl_absorpt_coefficient_mu 3.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.54253 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13703 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.1243 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 29.24 _reflns_number_total 4913 _reflns_number_gt 2564 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(3) _refine_ls_number_reflns 4913 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.791 _refine_ls_restrained_S_all 0.791 _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 1.01845(19) 0.50408(15) 0.15938(16) 0.0409(19) Uani 1 1 d G . . C2 C 0.99370(16) 0.46797(18) 0.17433(17) 0.061(2) Uani 1 1 d G . . H2 H 0.9632 0.4669 0.1692 0.073 Uiso 1 1 calc R . . C3 C 1.0145(2) 0.43342(15) 0.19695(18) 0.078(3) Uani 1 1 d G . . H3 H 0.9980 0.4093 0.2070 0.093 Uiso 1 1 calc R . . C4 C 1.0601(3) 0.4350(2) 0.20462(18) 0.082(3) Uani 1 1 d G . . H4 H 1.0741 0.4119 0.2198 0.099 Uiso 1 1 calc R . . C5 C 1.08488(16) 0.4711(3) 0.1897(2) 0.089(3) Uani 1 1 d G . . H5 H 1.1154 0.4721 0.1948 0.107 Uiso 1 1 calc R . . C6 C 1.06404(19) 0.50564(19) 0.16706(19) 0.072(3) Uani 1 1 d G . . H6 H 1.0806 0.5298 0.1571 0.086 Uiso 1 1 calc R . . C7 C 0.94040(17) 0.55774(17) 0.15640(17) 0.048(2) Uani 1 1 d G . . C8 C 0.9044(2) 0.57392(19) 0.13225(16) 0.062(2) Uani 1 1 d G . . H8 H 0.9060 0.5757 0.1014 0.075 Uiso 1 1 calc R . . C9 C 0.86604(17) 0.58748(19) 0.1542(3) 0.084(3) Uani 1 1 d G . . H9 H 0.8420 0.5983 0.1381 0.101 Uiso 1 1 calc R . . C10 C 0.86365(19) 0.58485(19) 0.2004(3) 0.091(3) Uani 1 1 d G . . H10 H 0.8380 0.5939 0.2151 0.109 Uiso 1 1 calc R . . C11 C 0.8996(3) 0.5687(2) 0.22449(17) 0.091(4) Uani 1 1 d G . . H11 H 0.8980 0.5669 0.2553 0.110 Uiso 1 1 calc R . . C12 C 0.9380(2) 0.5551(2) 0.20252(17) 0.070(3) Uani 1 1 d G . . H12 H 0.9621 0.5443 0.2187 0.083 Uiso 1 1 calc R . . C13 C 1.02359(19) 0.59685(15) 0.1386(2) 0.056(2) Uani 1 1 d G . . C14 C 1.03661(19) 0.6236(2) 0.10313(16) 0.056(2) Uani 1 1 d G . . H14 H 1.0305 0.6148 0.0741 0.067 Uiso 1 1 calc R . . C15 C 1.05880(19) 0.66336(19) 0.1111(2) 0.081(3) Uani 1 1 d G . . H15 H 1.0675 0.6812 0.0874 0.098 Uiso 1 1 calc R . . C16 C 1.0680(2) 0.67644(17) 0.1545(3) 0.089(4) Uani 1 1 d G . . H16 H 1.0828 0.7031 0.1598 0.106 Uiso 1 1 calc R . . C17 C 1.0550(3) 0.6497(2) 0.18994(19) 0.133(5) Uani 1 1 d G . . H17 H 1.0611 0.6585 0.2190 0.159 Uiso 1 1 calc R . . C18 C 1.0328(2) 0.6099(2) 0.18198(17) 0.107(4) Uani 1 1 d G . . H18 H 1.0241 0.5921 0.2057 0.128 Uiso 1 1 calc R . . C19 C 1.13969(13) 0.56968(17) -0.07587(17) 0.0379(18) Uani 1 1 d G . . C20 C 1.17160(18) 0.60244(14) -0.08280(17) 0.055(2) Uani 1 1 d G . . H20 H 1.1629 0.6310 -0.0909 0.066 Uiso 1 1 calc R . . C21 C 1.21647(16) 0.59247(19) -0.07760(19) 0.067(3) Uani 1 1 d G . . H21 H 1.2378 0.6144 -0.0822 0.080 Uiso 1 1 calc R . . C22 C 1.22943(14) 0.5498(2) -0.0655(2) 0.078(3) Uani 1 1 d G . . H22 H 1.2594 0.5431 -0.0620 0.094 Uiso 1 1 calc R . . C23 C 1.1975(2) 0.51700(16) -0.05856(19) 0.067(3) Uani 1 1 d G . . H23 H 1.2062 0.4884 -0.0505 0.081 Uiso 1 1 calc R . . C24 C 1.15264(18) 0.52696(15) -0.06376(19) 0.069(3) Uani 1 1 d G . . H24 H 1.1313 0.5050 -0.0591 0.083 Uiso 1 1 calc R . . I1 I 0.962345(16) 0.577905(16) -0.007881(16) 0.04474(13) Uani 1 1 d . . . I2 I 0.945976(16) 0.445976(16) 0.054024(16) 0.0490(2) Uani 1 3 d S . . Cu2 Cu 1.03719(3) 0.53719(3) -0.03719(3) 0.0529(4) Uani 1 3 d S . . Cu1 Cu 0.98833(4) 0.52432(3) 0.05556(3) 0.0578(3) Uani 1 1 d . . . P1 P 0.99209(7) 0.54690(7) 0.12680(6) 0.0439(5) Uani 1 1 d . . . P2 P 1.08062(6) 0.58062(6) -0.08062(6) 0.0410(8) Uani 1 3 d S . . 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 0.051(5) 0.038(4) 0.034(4) -0.008(4) 0.006(4) -0.006(4) C2 0.077(6) 0.050(5) 0.057(5) 0.003(5) -0.013(5) 0.008(5) C3 0.142(10) 0.048(6) 0.043(5) 0.016(4) -0.012(6) -0.020(6) C4 0.106(9) 0.086(8) 0.054(6) 0.009(6) -0.017(6) 0.042(7) C5 0.074(7) 0.109(9) 0.084(8) 0.028(7) -0.010(6) 0.007(7) C6 0.077(7) 0.073(7) 0.066(6) 0.007(6) 0.001(5) -0.009(6) C7 0.056(5) 0.044(5) 0.045(5) -0.006(4) 0.003(4) -0.002(4) C8 0.059(6) 0.064(6) 0.064(6) -0.004(5) 0.007(5) 0.006(5) C9 0.055(6) 0.076(7) 0.121(10) 0.009(7) -0.007(7) -0.012(6) C10 0.080(8) 0.056(6) 0.138(11) -0.021(7) 0.021(8) 0.004(6) C11 0.089(8) 0.091(8) 0.094(8) -0.036(7) 0.035(7) -0.002(6) C12 0.071(6) 0.094(7) 0.044(5) -0.011(5) 0.007(5) 0.009(6) C13 0.059(6) 0.049(5) 0.059(6) -0.007(5) 0.010(5) 0.009(4) C14 0.053(5) 0.055(6) 0.059(6) 0.011(5) -0.001(5) 0.002(5) C15 0.071(7) 0.053(6) 0.120(9) 0.039(6) -0.025(6) -0.015(5) C16 0.075(7) 0.051(6) 0.139(11) -0.042(7) 0.008(7) -0.021(5) C17 0.186(14) 0.114(10) 0.098(9) -0.036(8) 0.045(9) -0.093(10) C18 0.172(12) 0.095(8) 0.053(7) -0.016(6) 0.027(7) -0.068(8) C19 0.042(4) 0.044(5) 0.028(4) 0.005(4) 0.002(4) -0.007(4) C20 0.049(5) 0.057(5) 0.060(5) -0.011(5) -0.001(5) -0.019(5) C21 0.046(5) 0.069(7) 0.085(7) -0.017(5) 0.006(5) -0.013(5) C22 0.062(6) 0.089(8) 0.084(7) -0.016(6) -0.012(5) 0.024(6) C23 0.065(6) 0.055(6) 0.083(7) 0.004(5) 0.015(6) 0.021(5) C24 0.045(5) 0.078(7) 0.085(7) 0.034(6) 0.001(5) -0.001(5) I1 0.0445(3) 0.0429(3) 0.0468(3) 0.0032(2) 0.0001(3) 0.0032(3) I2 0.0490(2) 0.0490(2) 0.0490(2) 0.0050(3) 0.0050(3) -0.0050(3) Cu2 0.0529(4) 0.0529(4) 0.0529(4) 0.0058(5) 0.0058(5) -0.0058(5) Cu1 0.0780(8) 0.0553(6) 0.0401(6) 0.0008(5) -0.0035(5) 0.0002(6) P1 0.0532(13) 0.0428(13) 0.0356(11) -0.0023(10) -0.0007(10) -0.0063(10) P2 0.0410(8) 0.0410(8) 0.0410(8) 0.0040(10) 0.0040(10) -0.0040(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 P1 1.801(5) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C7 P1 1.819(5) . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C13 P1 1.809(4) . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C19 P2 1.811(4) . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? I1 Cu1 2.6148(11) . ? I1 Cu2 2.7076(9) . ? I1 Cu1 2.7891(12) 42_545 ? I2 Cu1 2.6768(12) 35 ? I2 Cu1 2.6768(12) . ? I2 Cu1 2.6768(12) 42_545 ? Cu2 P2 2.260(4) . ? Cu2 I1 2.7077(9) 35 ? Cu2 I1 2.7078(9) 42_545 ? Cu1 P1 2.249(2) . ? Cu1 I1 2.7889(12) 35 ? Cu1 Cu1 2.9450(17) 35 ? Cu1 Cu1 2.9451(17) 42_545 ? P2 C19 1.811(4) 42_545 ? P2 C19 1.811(4) 35 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.0 . . ? C2 C1 P1 119.9(4) . . ? C6 C1 P1 120.0(4) . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 P1 118.1(4) . . ? C12 C7 P1 121.4(4) . . ? C7 C8 C9 120.0 . . ? C10 C9 C8 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 P1 118.4(4) . . ? C18 C13 P1 121.5(4) . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 P2 122.4(3) . . ? C24 C19 P2 117.6(3) . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? Cu1 I1 Cu2 73.19(4) . . ? Cu1 I1 Cu1 65.95(4) . 42_545 ? Cu2 I1 Cu1 70.52(4) . 42_545 ? Cu1 I2 Cu1 66.75(4) 35 . ? Cu1 I2 Cu1 66.75(4) 35 42_545 ? Cu1 I2 Cu1 66.75(4) . 42_545 ? P2 Cu2 I1 113.98(4) . . ? P2 Cu2 I1 113.99(4) . 35 ? I1 Cu2 I1 104.60(4) . 35 ? P2 Cu2 I1 113.99(4) . 42_545 ? I1 Cu2 I1 104.61(4) . 42_545 ? I1 Cu2 I1 104.60(4) 35 42_545 ? P1 Cu1 I1 121.56(7) . . ? P1 Cu1 I2 107.80(6) . . ? I1 Cu1 I2 112.77(4) . . ? P1 Cu1 I1 100.88(7) . 35 ? I1 Cu1 I1 104.87(4) . 35 ? I2 Cu1 I1 107.44(4) . 35 ? P1 Cu1 Cu1 130.85(8) . 35 ? I1 Cu1 Cu1 106.56(3) . 35 ? I2 Cu1 Cu1 56.625(19) . 35 ? I1 Cu1 Cu1 54.18(4) 35 35 ? P1 Cu1 Cu1 155.42(7) . 42_545 ? I1 Cu1 Cu1 59.87(4) . 42_545 ? I2 Cu1 Cu1 56.626(19) . 42_545 ? I1 Cu1 Cu1 102.12(3) 35 42_545 ? Cu1 Cu1 Cu1 60.0 35 42_545 ? C1 P1 C13 104.9(3) . . ? C1 P1 C7 103.7(3) . . ? C13 P1 C7 101.7(3) . . ? C1 P1 Cu1 108.91(18) . . ? C13 P1 Cu1 117.6(2) . . ? C7 P1 Cu1 118.5(2) . . ? C19 P2 C19 103.9(2) 42_545 . ? C19 P2 C19 103.9(2) 42_545 35 ? C19 P2 C19 103.9(2) . 35 ? C19 P2 Cu2 114.57(19) 42_545 . ? C19 P2 Cu2 114.57(19) . . ? C19 P2 Cu2 114.56(19) 35 . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.794 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.081 # Attachment '- [CuI(PPh3)2]1.5_CH2Cl2.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-07-29 at 17:34:28 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : zhou100k struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# #TrackingRef '- [CuI(PPh3)2]1.5_CH2Cl2.cif' #------------------ AUDIT DETAILS -------------------------------------------# #------------------ AUTHOR DETAILS -------------------------------------------# data_zhou100k _database_code_depnum_ccdc_archive 'CCDC 838122' #TrackingRef '- [CuI(PPh3)2]1.5_CH2Cl2.cif' _audit_creation_date 2011-07-29T17:34:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C55 H47 Cl2 Cu2 I2 P3' _chemical_formula_sum 'C55 H47 Cl2 Cu2 I2 P3' _chemical_formula_weight 1252.62 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 15.7252(6) _cell_length_b 19.5305(7) _cell_length_c 17.6410(8) _cell_angle_alpha 90 _cell_angle_beta 110.473(5) _cell_angle_gamma 90 _cell_volume 5075.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8337 _cell_measurement_theta_min 2.6711 _cell_measurement_theta_max 29.0272 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.291 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_unetI/netI 0.1024 _diffrn_reflns_number 32388 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 29.09 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.944 _diffrn_measured_fraction_theta_max 0.821 _reflns_number_total 11167 _reflns_number_gt 6729 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11167 _refine_ls_number_parameters 577 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1644 _refine_ls_R_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.3689 _refine_ls_wR_factor_gt 0.3235 _refine_ls_goodness_of_fit_ref 1.233 _refine_ls_restrained_S_all 1.232 _refine_ls_shift/su_max 0.17 _refine_ls_shift/su_mean 0.006 _refine_diff_density_max 2.749 _refine_diff_density_min -3.715 _refine_diff_density_rms 0.268 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' I I -0.4742 1.8119 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3470(7) -0.0652(5) 0.4903(6) 0.021(2) Uani 1 1 d . . . C2 C 0.3967(7) -0.1062(6) 0.4605(9) 0.037(3) Uani 1 1 d . . . H2 H 0.3673 -0.1301 0.4129 0.044 Uiso 1 1 calc R . . C3 C 0.4904(8) -0.1143(7) 0.4976(9) 0.043(3) Uani 1 1 d . . . H3 H 0.5233 -0.1423 0.4752 0.051 Uiso 1 1 calc R . . C4 C 0.5332(8) -0.0786(7) 0.5700(9) 0.041(3) Uani 1 1 d . . . H4 H 0.5955 -0.0822 0.5966 0.049 Uiso 1 1 calc R . . C5 C 0.4825(9) -0.0389(7) 0.6007(8) 0.041(3) Uani 1 1 d . . . H5 H 0.5118 -0.0172 0.6499 0.049 Uiso 1 1 calc R . . C6 C 0.3911(8) -0.0285(7) 0.5645(8) 0.040(3) Uani 1 1 d . . . H6 H 0.3592 0.0008 0.5865 0.048 Uiso 1 1 calc R . . C7 C 0.1881(6) 0.0161(5) 0.4783(7) 0.021(2) Uani 1 1 d . . . C8 C 0.2186(8) 0.0796(6) 0.4595(8) 0.036(3) Uani 1 1 d . . . H8 H 0.258 0.0805 0.4307 0.043 Uiso 1 1 calc R . . C9 C 0.1912(8) 0.1400(6) 0.4829(9) 0.041(3) Uani 1 1 d . . . H9 H 0.2122 0.1814 0.4703 0.049 Uiso 1 1 calc R . . C10 C 0.1303(8) 0.1392(6) 0.5269(8) 0.038(3) Uani 1 1 d . . . H10 H 0.113 0.18 0.5445 0.046 Uiso 1 1 calc R . . C11 C 0.0978(8) 0.0785(6) 0.5429(7) 0.033(3) Uani 1 1 d . . . H11 H 0.0557 0.0783 0.5691 0.04 Uiso 1 1 calc R . . C12 C 0.1276(7) 0.0142(6) 0.5198(7) 0.025(2) Uani 1 1 d . . . H12 H 0.1068 -0.0273 0.5324 0.03 Uiso 1 1 calc R . . C13 C 0.1833(6) -0.1303(5) 0.4882(7) 0.020(2) Uani 1 1 d . . . C14 C 0.2267(8) -0.1478(6) 0.5697(7) 0.032(3) Uani 1 1 d . . . H14 H 0.2777 -0.1235 0.6011 0.038 Uiso 1 1 calc R . . C15 C 0.1939(9) -0.2018(6) 0.6042(8) 0.034(3) Uani 1 1 d . . . H15 H 0.2228 -0.2127 0.6585 0.041 Uiso 1 1 calc R . . C16 C 0.1187(8) -0.2388(5) 0.5579(8) 0.032(3) Uani 1 1 d . . . H16 H 0.0969 -0.2745 0.5808 0.038 Uiso 1 1 calc R . . C17 C 0.0757(8) -0.2219(6) 0.4764(9) 0.035(3) Uani 1 1 d . . . H17 H 0.0242 -0.2456 0.4448 0.042 Uiso 1 1 calc R . . C18 C 0.1108(7) -0.1693(5) 0.4427(7) 0.026(2) Uani 1 1 d . . . H18 H 0.0841 -0.1602 0.3877 0.031 Uiso 1 1 calc R . . C19 C -0.0470(6) -0.0045(5) 0.2229(6) 0.0171(19) Uani 1 1 d . . . C20 C -0.0190(7) 0.0341(5) 0.2948(7) 0.024(2) Uani 1 1 d . . . H20 H 0.0322 0.0209 0.3379 0.028 Uiso 1 1 calc R . . C21 C -0.0676(8) 0.0920(6) 0.3019(8) 0.032(3) Uani 1 1 d . . . H21 H -0.0496 0.1177 0.3493 0.038 Uiso 1 1 calc R . . C22 C -0.1443(7) 0.1104(6) 0.2356(8) 0.031(3) Uani 1 1 d . . . H22 H -0.1766 0.1495 0.2391 0.037 Uiso 1 1 calc R . . C23 C -0.1721(8) 0.0738(5) 0.1681(8) 0.028(2) Uani 1 1 d . . . H23 H -0.224 0.0871 0.1257 0.034 Uiso 1 1 calc R . . C24 C -0.1244(6) 0.0156(5) 0.1598(6) 0.020(2) Uani 1 1 d . . . H24 H -0.1446 -0.0096 0.1121 0.024 Uiso 1 1 calc R . . C25 C -0.0479(6) -0.1506(5) 0.2363(6) 0.0163(19) Uani 1 1 d . . . C26 C -0.1284(7) -0.1421(6) 0.2525(7) 0.026(2) Uani 1 1 d . . . H26 H -0.1492 -0.098 0.2558 0.031 Uiso 1 1 calc R . . C27 C -0.1774(7) -0.1971(6) 0.2637(8) 0.031(3) Uani 1 1 d . . . H27 H -0.231 -0.1902 0.2738 0.037 Uiso 1 1 calc R . . C28 C -0.1461(8) -0.2628(6) 0.2599(7) 0.034(3) Uani 1 1 d . . . H28 H -0.178 -0.3003 0.2685 0.04 Uiso 1 1 calc R . . C29 C -0.0704(9) -0.2722(6) 0.2441(8) 0.037(3) Uani 1 1 d . . . H29 H -0.0514 -0.3167 0.24 0.045 Uiso 1 1 calc R . . C30 C -0.0181(8) -0.2175(5) 0.2331(8) 0.033(3) Uani 1 1 d . . . H30 H 0.0357 -0.2256 0.2239 0.039 Uiso 1 1 calc R . . C31 C 0.0029(6) -0.0903(5) 0.1113(6) 0.020(2) Uani 1 1 d . . . C32 C -0.0743(7) -0.1230(5) 0.0560(7) 0.027(2) Uani 1 1 d . . . H32 H -0.1184 -0.1398 0.075 0.032 Uiso 1 1 calc R . . C33 C -0.0868(7) -0.1308(6) -0.0246(7) 0.027(2) Uani 1 1 d . . . H33 H -0.1386 -0.1519 -0.0599 0.032 Uiso 1 1 calc R . . C34 C -0.0172(8) -0.1054(6) -0.0526(7) 0.032(3) Uani 1 1 d . . . H34 H -0.0237 -0.1089 -0.1069 0.038 Uiso 1 1 calc R . . C35 C 0.0576(7) -0.0765(5) 0.0008(6) 0.023(2) Uani 1 1 d . . . H35 H 0.1039 -0.0622 -0.0169 0.027 Uiso 1 1 calc R . . C36 C 0.0677(6) -0.0671(5) 0.0825(6) 0.023(2) Uani 1 1 d . . . H36 H 0.1188 -0.045 0.1172 0.028 Uiso 1 1 calc R . . C37 C 0.3536(6) 0.0419(6) 0.0703(7) 0.026(2) Uani 1 1 d . . . C38 C 0.3395(7) 0.0452(7) -0.0138(7) 0.033(3) Uani 1 1 d . . . H38 H 0.3406 0.0054 -0.0425 0.04 Uiso 1 1 calc R . . C39 C 0.3241(7) 0.1076(7) -0.0526(8) 0.035(3) Uani 1 1 d . . . H39 H 0.3156 0.1094 -0.1075 0.042 Uiso 1 1 calc R . . C40 C 0.3209(8) 0.1673(7) -0.0125(9) 0.042(3) Uani 1 1 d . . . H40 H 0.3108 0.209 -0.0395 0.051 Uiso 1 1 calc R . . C41 C 0.3329(10) 0.1641(6) 0.0690(9) 0.042(3) Uani 1 1 d . . . H41 H 0.3297 0.2041 0.0964 0.051 Uiso 1 1 calc R . . C42 C 0.3495(8) 0.1035(7) 0.1099(8) 0.040(3) Uani 1 1 d . . . H42 H 0.3583 0.103 0.1648 0.048 Uiso 1 1 calc R . . C43 C 0.4951(7) -0.0337(7) 0.1862(7) 0.051(4) Uani 1 1 d D . . C44 C 0.5517(8) 0.0205(9) 0.1795(8) 0.084(7) Uani 1 1 d D . . H44 H 0.5308 0.0574 0.1447 0.101 Uiso 1 1 calc R . . C45 C 0.6436(9) 0.0131(13) 0.2312(9) 0.152(15) Uani 1 1 d D . . H45 H 0.6843 0.0476 0.231 0.182 Uiso 1 1 calc R . . C46 C 0.6771(13) -0.0435(12) 0.2829(11) 0.135(14) Uani 1 1 d D . . H46 H 0.7387 -0.046 0.313 0.162 Uiso 1 1 calc R . . C47 C 0.6196(10) -0.0958(11) 0.2898(11) 0.125(12) Uani 1 1 d D . . H47 H 0.641 -0.1326 0.3249 0.15 Uiso 1 1 calc R . . C48 C 0.5271(10) -0.0897(7) 0.2404(8) 0.071(6) Uani 1 1 d D . . H48 H 0.4862 -0.123 0.2435 0.086 Uiso 1 1 calc R . . C49 C 0.3690(6) -0.1052(6) 0.0559(7) 0.025(2) Uani 1 1 d . . . C50 C 0.4368(7) -0.1109(6) 0.0190(8) 0.033(3) Uani 1 1 d . . . H50 H 0.4848 -0.08 0.0321 0.04 Uiso 1 1 calc R . . C51 C 0.4301(8) -0.1618(6) -0.0353(7) 0.031(3) Uani 1 1 d . . . H51 H 0.4756 -0.1672 -0.0573 0.037 Uiso 1 1 calc R . . C52 C 0.3566(7) -0.2055(6) -0.0580(7) 0.029(2) Uani 1 1 d . . . H52 H 0.3517 -0.2388 -0.097 0.035 Uiso 1 1 calc R . . C53 C 0.2908(7) -0.2006(6) -0.0242(7) 0.031(3) Uani 1 1 d . . . H53 H 0.2415 -0.2303 -0.0399 0.037 Uiso 1 1 calc R . . C54 C 0.2987(7) -0.1505(5) 0.0342(7) 0.026(2) Uani 1 1 d . . . H54 H 0.2553 -0.1479 0.0588 0.031 Uiso 1 1 calc R . . C55 C 0.5285(15) 0.2252(9) 0.3404(12) 0.083(6) Uani 1 1 d . . . H55A H 0.558 0.2679 0.3629 0.099 Uiso 1 1 calc R . . H55B H 0.5512 0.1897 0.3808 0.099 Uiso 1 1 calc R . . Cl1 Cl 0.5526(4) 0.2043(5) 0.2534(4) 0.131(3) Uani 1 1 d . . . Cl2 Cl 0.4081(4) 0.2336(2) 0.3141(3) 0.0836(15) Uani 1 1 d . . . Cu1 Cu 0.16730(7) -0.06952(6) 0.30251(7) 0.0173(3) Uani 1 1 d . . . Cu2 Cu 0.29302(9) -0.05187(7) 0.20648(9) 0.0277(4) Uani 1 1 d . . . I1 I 0.25610(8) -0.16360(6) 0.25317(6) 0.0591(4) Uani 1 1 d . . . I2 I 0.22784(6) 0.04744(5) 0.25729(6) 0.0446(3) Uani 1 1 d . . . P1 P 0.22307(16) -0.06159(13) 0.43970(17) 0.0191(6) Uani 1 1 d . . . P2 P 0.02023(16) -0.07980(13) 0.21907(16) 0.0174(5) Uani 1 1 d . . . P3 P 0.37448(17) -0.03684(16) 0.12839(18) 0.0256(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(5) 0.026(5) 0.020(5) 0.003(4) 0.012(4) -0.003(4) C2 0.018(5) 0.035(6) 0.055(8) -0.011(6) 0.011(5) 0.001(5) C3 0.016(5) 0.056(8) 0.050(8) -0.005(7) 0.003(5) 0.001(5) C4 0.017(5) 0.053(8) 0.049(8) 0.010(7) 0.006(5) -0.005(5) C5 0.035(6) 0.052(8) 0.025(7) -0.005(6) -0.002(5) -0.003(6) C6 0.023(5) 0.062(8) 0.034(7) -0.007(6) 0.009(5) 0.004(6) C7 0.008(4) 0.023(5) 0.031(6) -0.013(4) 0.004(4) -0.003(4) C8 0.035(6) 0.030(6) 0.054(8) -0.015(6) 0.028(6) -0.002(5) C9 0.034(6) 0.026(6) 0.069(10) -0.014(6) 0.027(7) -0.002(5) C10 0.042(7) 0.026(6) 0.036(7) -0.020(5) -0.001(6) 0.018(5) C11 0.030(6) 0.046(7) 0.027(6) -0.002(6) 0.014(5) 0.017(5) C12 0.019(5) 0.033(6) 0.025(6) 0.005(5) 0.011(4) 0.008(4) C13 0.017(4) 0.023(5) 0.024(5) -0.001(4) 0.012(4) 0.003(4) C14 0.036(6) 0.038(6) 0.027(6) -0.015(5) 0.017(5) 0.005(5) C15 0.052(7) 0.030(6) 0.029(7) -0.001(5) 0.024(6) 0.006(5) C16 0.044(7) 0.019(5) 0.043(8) 0.006(5) 0.028(6) 0.007(5) C17 0.024(5) 0.026(6) 0.061(9) 0.003(6) 0.021(6) 0.001(4) C18 0.022(5) 0.025(5) 0.029(6) 0.009(5) 0.007(5) 0.003(4) C19 0.016(4) 0.019(4) 0.020(5) 0.006(4) 0.012(4) 0.002(4) C20 0.017(4) 0.026(5) 0.031(6) -0.014(5) 0.013(4) -0.004(4) C21 0.039(6) 0.021(5) 0.043(7) -0.008(5) 0.025(6) 0.002(5) C22 0.027(5) 0.032(6) 0.039(7) 0.003(5) 0.019(5) 0.012(5) C23 0.029(5) 0.025(5) 0.033(6) -0.002(5) 0.015(5) 0.009(4) C24 0.021(5) 0.024(5) 0.017(5) 0.006(4) 0.010(4) 0.001(4) C25 0.015(4) 0.019(4) 0.014(5) -0.002(4) 0.004(4) -0.007(4) C26 0.023(5) 0.029(5) 0.031(6) -0.001(5) 0.018(5) 0.001(4) C27 0.022(5) 0.034(6) 0.041(7) -0.005(5) 0.017(5) 0.007(5) C28 0.040(6) 0.029(6) 0.030(7) 0.001(5) 0.011(5) -0.009(5) C29 0.047(7) 0.021(5) 0.049(8) 0.000(5) 0.025(7) -0.003(5) C30 0.037(6) 0.019(5) 0.048(8) -0.001(5) 0.022(6) 0.009(4) C31 0.017(4) 0.025(5) 0.019(5) 0.002(4) 0.007(4) 0.012(4) C32 0.020(5) 0.029(5) 0.031(6) -0.013(5) 0.007(4) 0.006(4) C33 0.022(5) 0.031(6) 0.021(6) -0.004(5) 0.000(4) 0.005(4) C34 0.038(6) 0.026(5) 0.022(6) -0.003(5) -0.001(5) 0.015(5) C35 0.025(5) 0.029(5) 0.023(5) 0.006(5) 0.019(4) 0.013(4) C36 0.014(4) 0.034(6) 0.018(5) -0.005(5) 0.003(4) 0.010(4) C37 0.012(4) 0.038(6) 0.032(6) -0.011(5) 0.012(4) -0.007(4) C38 0.021(5) 0.058(8) 0.022(6) -0.006(6) 0.009(5) 0.000(5) C39 0.021(5) 0.054(8) 0.027(6) 0.010(6) 0.003(5) 0.000(5) C40 0.026(6) 0.051(8) 0.049(9) 0.004(7) 0.013(6) 0.002(6) C41 0.055(8) 0.031(6) 0.049(9) -0.007(6) 0.030(7) -0.016(6) C42 0.043(7) 0.049(7) 0.033(7) -0.012(6) 0.020(6) -0.025(6) C43 0.019(5) 0.099(11) 0.030(7) -0.029(8) 0.003(5) 0.013(7) C44 0.032(7) 0.19(2) 0.042(9) -0.031(12) 0.026(7) -0.035(10) C45 0.024(8) 0.38(5) 0.059(13) -0.10(2) 0.030(9) -0.044(16) C46 0.044(10) 0.29(4) 0.058(13) -0.112(19) 0.001(10) 0.065(16) C47 0.066(12) 0.16(2) 0.091(16) -0.091(16) -0.053(12) 0.086(14) C48 0.072(10) 0.077(11) 0.036(8) -0.031(8) -0.017(8) 0.056(9) C49 0.017(4) 0.042(6) 0.021(5) -0.003(5) 0.014(4) -0.003(4) C50 0.021(5) 0.043(7) 0.043(7) -0.005(6) 0.022(5) 0.000(5) C51 0.033(6) 0.045(7) 0.024(6) -0.009(5) 0.022(5) 0.001(5) C52 0.026(5) 0.030(6) 0.029(6) 0.003(5) 0.009(5) 0.005(5) C53 0.026(5) 0.031(6) 0.034(7) 0.004(5) 0.010(5) -0.005(5) C54 0.026(5) 0.030(5) 0.029(6) 0.009(5) 0.018(5) -0.001(4) C55 0.122(18) 0.050(10) 0.071(13) 0.001(9) 0.027(13) -0.040(10) Cl1 0.063(3) 0.259(9) 0.068(4) -0.047(5) 0.017(3) -0.049(4) Cl2 0.079(3) 0.067(3) 0.085(4) 0.009(3) 0.004(3) 0.031(2) Cu1 0.0146(5) 0.0223(6) 0.0168(6) -0.0029(5) 0.0079(5) 0.0011(5) Cu2 0.0196(6) 0.0455(8) 0.0217(7) 0.0028(6) 0.0116(6) 0.0065(6) I1 0.0747(8) 0.0598(7) 0.0436(6) -0.0004(5) 0.0218(5) 0.0152(5) I2 0.0406(5) 0.0489(6) 0.0441(6) -0.0028(4) 0.0146(4) -0.0039(4) P1 0.0148(11) 0.0238(13) 0.0199(14) -0.0039(11) 0.0076(10) -0.0007(10) P2 0.0153(11) 0.0197(12) 0.0189(13) -0.0042(10) 0.0081(10) 0.0014(9) P3 0.0154(12) 0.0435(16) 0.0206(15) -0.0011(13) 0.0097(11) 0.0012(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.348(15) . ? C1 C6 1.439(17) . ? C1 P1 1.839(10) . ? C2 C3 1.396(15) . ? C3 C4 1.404(19) . ? C4 C5 1.352(19) . ? C5 C6 1.368(17) . ? C7 C12 1.388(14) . ? C7 C8 1.412(16) . ? C7 P1 1.825(10) . ? C8 C9 1.367(16) . ? C9 C10 1.427(18) . ? C10 C11 1.358(18) . ? C11 C12 1.448(16) . ? C13 C18 1.373(14) . ? C13 C14 1.401(16) . ? C13 P1 1.816(10) . ? C14 C15 1.404(17) . ? C15 C16 1.382(18) . ? C16 C17 1.398(19) . ? C17 C18 1.393(15) . ? C19 C24 1.388(13) . ? C19 C20 1.408(14) . ? C19 P2 1.826(10) . ? C20 C21 1.395(14) . ? C21 C22 1.402(17) . ? C22 C23 1.326(17) . ? C23 C24 1.397(14) . ? C25 C30 1.395(14) . ? C25 C26 1.402(13) . ? C25 P2 1.840(9) . ? C26 C27 1.376(16) . ? C27 C28 1.385(16) . ? C28 C29 1.327(17) . ? C29 C30 1.403(16) . ? C31 C36 1.365(14) . ? C31 C32 1.415(14) . ? C31 P2 1.835(11) . ? C32 C33 1.375(16) . ? C33 C34 1.438(17) . ? C34 C35 1.347(16) . ? C35 C36 1.405(15) . ? C37 C42 1.403(16) . ? C37 C38 1.424(17) . ? C37 P3 1.814(12) . ? C38 C39 1.377(17) . ? C39 C40 1.373(19) . ? C40 C41 1.38(2) . ? C41 C42 1.362(18) . ? C43 C44 1.414(9) . ? C43 C48 1.423(9) . ? C43 P3 1.814(11) . ? C44 C45 1.421(9) . ? C45 C46 1.412(10) . ? C46 C47 1.397(10) . ? C47 C48 1.415(9) . ? C49 C54 1.361(14) . ? C49 C50 1.434(13) . ? C49 P3 1.830(11) . ? C50 C51 1.360(16) . ? C51 C52 1.379(16) . ? C52 C53 1.367(15) . ? C53 C54 1.395(16) . ? C55 Cl1 1.75(2) . ? C55 Cl2 1.79(2) . ? Cu1 P1 2.273(3) . ? Cu1 P2 2.275(3) . ? Cu1 I1 2.6331(15) . ? Cu1 I2 2.7003(15) . ? Cu1 Cu2 3.0396(18) . ? Cu2 P3 2.204(3) . ? Cu2 I1 2.4721(18) . ? Cu2 I2 2.5016(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.3(10) . . ? C2 C1 P1 119.6(9) . . ? C6 C1 P1 121.0(8) . . ? C1 C2 C3 123.1(12) . . ? C2 C3 C4 117.4(12) . . ? C5 C4 C3 119.2(11) . . ? C4 C5 C6 124.6(12) . . ? C5 C6 C1 116.4(11) . . ? C12 C7 C8 119.8(9) . . ? C12 C7 P1 121.8(8) . . ? C8 C7 P1 118.2(8) . . ? C9 C8 C7 121.2(11) . . ? C8 C9 C10 119.8(11) . . ? C11 C10 C9 119.7(10) . . ? C10 C11 C12 121.0(11) . . ? C7 C12 C11 118.4(10) . . ? C18 C13 C14 118.1(10) . . ? C18 C13 P1 119.2(8) . . ? C14 C13 P1 122.6(8) . . ? C13 C14 C15 120.5(11) . . ? C16 C15 C14 120.3(12) . . ? C15 C16 C17 119.4(11) . . ? C18 C17 C16 119.4(11) . . ? C13 C18 C17 122.2(11) . . ? C24 C19 C20 118.8(9) . . ? C24 C19 P2 123.7(8) . . ? C20 C19 P2 117.5(7) . . ? C21 C20 C19 120.4(10) . . ? C20 C21 C22 118.1(11) . . ? C23 C22 C21 121.9(10) . . ? C22 C23 C24 120.8(11) . . ? C19 C24 C23 119.9(10) . . ? C30 C25 C26 117.4(9) . . ? C30 C25 P2 118.3(8) . . ? C26 C25 P2 124.3(7) . . ? C27 C26 C25 121.8(10) . . ? C26 C27 C28 119.4(10) . . ? C29 C28 C27 119.9(11) . . ? C28 C29 C30 122.4(11) . . ? C25 C30 C29 119.1(10) . . ? C36 C31 C32 117.7(10) . . ? C36 C31 P2 119.2(8) . . ? C32 C31 P2 123.1(8) . . ? C33 C32 C31 122.8(11) . . ? C32 C33 C34 117.8(10) . . ? C35 C34 C33 119.2(11) . . ? C34 C35 C36 121.9(10) . . ? C31 C36 C35 120.5(10) . . ? C42 C37 C38 117.6(12) . . ? C42 C37 P3 118.5(9) . . ? C38 C37 P3 123.9(9) . . ? C39 C38 C37 119.6(12) . . ? C40 C39 C38 121.7(12) . . ? C39 C40 C41 118.8(13) . . ? C42 C41 C40 121.3(13) . . ? C41 C42 C37 121.0(12) . . ? C44 C43 C48 123.1(13) . . ? C44 C43 P3 122.9(9) . . ? C48 C43 P3 114.0(9) . . ? C43 C44 C45 113.5(15) . . ? C46 C45 C44 124.0(17) . . ? C47 C46 C45 121.5(17) . . ? C46 C47 C48 116.1(17) . . ? C47 C48 C43 121.6(16) . . ? C54 C49 C50 118.8(10) . . ? C54 C49 P3 120.4(8) . . ? C50 C49 P3 120.8(8) . . ? C51 C50 C49 119.4(10) . . ? C50 C51 C52 120.5(10) . . ? C53 C52 C51 121.0(11) . . ? C52 C53 C54 119.1(10) . . ? C49 C54 C53 121.2(10) . . ? Cl1 C55 Cl2 109.1(11) . . ? P1 Cu1 P2 128.42(10) . . ? P1 Cu1 I1 110.36(8) . . ? P2 Cu1 I1 105.14(8) . . ? P1 Cu1 I2 102.26(8) . . ? P2 Cu1 I2 105.49(8) . . ? I1 Cu1 I2 102.13(5) . . ? P1 Cu1 Cu2 120.12(8) . . ? P2 Cu1 Cu2 111.20(8) . . ? I1 Cu1 Cu2 51.06(4) . . ? I2 Cu1 Cu2 51.26(4) . . ? P3 Cu2 I1 125.53(10) . . ? P3 Cu2 I2 121.41(10) . . ? I1 Cu2 I2 113.06(6) . . ? P3 Cu2 Cu1 175.39(10) . . ? I1 Cu2 Cu1 55.94(4) . . ? I2 Cu2 Cu1 57.35(4) . . ? Cu2 I1 Cu1 73.00(5) . . ? Cu2 I2 Cu1 71.39(5) . . ? C13 P1 C7 103.9(5) . . ? C13 P1 C1 102.9(4) . . ? C7 P1 C1 104.9(4) . . ? C13 P1 Cu1 112.5(4) . . ? C7 P1 Cu1 113.6(4) . . ? C1 P1 Cu1 117.6(3) . . ? C19 P2 C31 104.5(4) . . ? C19 P2 C25 102.8(4) . . ? C31 P2 C25 101.7(5) . . ? C19 P2 Cu1 112.1(3) . . ? C31 P2 Cu1 115.4(3) . . ? C25 P2 Cu1 118.6(3) . . ? C43 P3 C37 103.7(5) . . ? C43 P3 C49 101.6(5) . . ? C37 P3 C49 105.6(5) . . ? C43 P3 Cu2 112.0(4) . . ? C37 P3 Cu2 115.8(3) . . ? C49 P3 Cu2 116.4(3) . . ? # END of CIF # Attachment '- monomero_b_RT.cif' data_shelxl4 _database_code_depnum_ccdc_archive 'CCDC 838123' #TrackingRef '- monomero_b_RT.cif' _audit_update_record ; 2011-06-28 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H45 Cu I P3' _chemical_formula_weight 977.25 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' Cu Cu 0.3201 1.2651 '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' 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 'P 1 21/c 1' 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 13.2375(5) _cell_length_b 18.5976(7) _cell_length_c 18.9297(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.953(4) _cell_angle_gamma 90.00 _cell_volume 4649.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7743 _cell_measurement_theta_min 2.6740 _cell_measurement_theta_max 28.9608 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 1.272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95037 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 293(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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1340 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24269 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0876 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 29.02 _reflns_number_total 10549 _reflns_number_gt 5638 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0872P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10549 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 0.763 _refine_ls_restrained_S_all 0.763 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.49785(15) 0.41363(14) 0.14472(15) 0.0381(9) Uani 1 1 d G . . C2 C 0.51372(19) 0.34000(13) 0.15146(16) 0.0468(11) Uani 1 1 d G . . H2 H 0.4591 0.3093 0.1559 0.056 Uiso 1 1 calc R . . C3 C 0.6112(2) 0.31228(12) 0.15159(16) 0.0571(13) Uani 1 1 d G . . H3 H 0.6219 0.2630 0.1561 0.068 Uiso 1 1 calc R . . C4 C 0.69290(17) 0.35819(18) 0.14496(17) 0.0594(13) Uani 1 1 d G . . H4 H 0.7582 0.3396 0.1450 0.071 Uiso 1 1 calc R . . C5 C 0.67704(17) 0.43183(16) 0.13822(17) 0.0615(13) Uani 1 1 d G . . H5 H 0.7317 0.4625 0.1338 0.074 Uiso 1 1 calc R . . C6 C 0.5795(2) 0.45955(11) 0.13809(16) 0.0499(11) Uani 1 1 d G . . H6 H 0.5689 0.5088 0.1336 0.060 Uiso 1 1 calc R . . C7 C 0.31935(19) 0.41431(14) 0.05214(11) 0.0360(9) Uani 1 1 d G . . C8 C 0.21552(18) 0.41628(16) 0.03525(14) 0.0491(11) Uani 1 1 d G . . H8 H 0.1720 0.4316 0.0688 0.059 Uiso 1 1 calc R . . C9 C 0.17669(16) 0.39543(18) -0.03172(16) 0.0652(14) Uani 1 1 d G . . H9 H 0.1072 0.3967 -0.0430 0.078 Uiso 1 1 calc R . . C10 C 0.2417(2) 0.37260(17) -0.08181(12) 0.0623(14) Uani 1 1 d G . . H10 H 0.2157 0.3586 -0.1266 0.075 Uiso 1 1 calc R . . C11 C 0.3455(2) 0.37063(16) -0.06493(13) 0.0556(12) Uani 1 1 d G . . H11 H 0.3890 0.3554 -0.0984 0.067 Uiso 1 1 calc R . . C12 C 0.38436(15) 0.39149(15) 0.00204(14) 0.0488(11) Uani 1 1 d G . . H12 H 0.4538 0.3902 0.0133 0.059 Uiso 1 1 calc R . . C13 C 0.3777(2) 0.54282(10) 0.12798(13) 0.0392(10) Uani 1 1 d G . . C14 C 0.3501(2) 0.57611(13) 0.06378(12) 0.0448(10) Uani 1 1 d G . . H14 H 0.3267 0.5487 0.0249 0.054 Uiso 1 1 calc R . . C15 C 0.3574(3) 0.65037(14) 0.05764(14) 0.0603(13) Uani 1 1 d G . . H15 H 0.3390 0.6726 0.0147 0.072 Uiso 1 1 calc R . . C16 C 0.3923(3) 0.69135(10) 0.11571(18) 0.0732(16) Uani 1 1 d G . . H16 H 0.3972 0.7410 0.1116 0.088 Uiso 1 1 calc R . . C17 C 0.4199(3) 0.65806(14) 0.17990(15) 0.0750(17) Uani 1 1 d G . . H17 H 0.4432 0.6855 0.2187 0.090 Uiso 1 1 calc R . . C18 C 0.4125(3) 0.58380(15) 0.18604(11) 0.0592(13) Uani 1 1 d G . . H18 H 0.4310 0.5615 0.2290 0.071 Uiso 1 1 calc R . . C19 C 0.3136(2) 0.52688(12) 0.38274(14) 0.0419(10) Uani 1 1 d G . . C20 C 0.2702(2) 0.57731(15) 0.33568(11) 0.0520(12) Uani 1 1 d G . . H20 H 0.2628 0.5670 0.2875 0.062 Uiso 1 1 calc R . . C21 C 0.2380(2) 0.64318(13) 0.36058(16) 0.0590(13) Uani 1 1 d G . . H21 H 0.2090 0.6769 0.3291 0.071 Uiso 1 1 calc R . . C22 C 0.2492(3) 0.65861(13) 0.43254(17) 0.0622(14) Uani 1 1 d G . . H22 H 0.2277 0.7027 0.4492 0.075 Uiso 1 1 calc R . . C23 C 0.2926(3) 0.60819(17) 0.47960(12) 0.0726(16) Uani 1 1 d G . . H23 H 0.3000 0.6185 0.5277 0.087 Uiso 1 1 calc R . . C24 C 0.3248(2) 0.54232(15) 0.45470(13) 0.0601(13) Uani 1 1 d G . . H24 H 0.3538 0.5086 0.4862 0.072 Uiso 1 1 calc R . . C25 C 0.49128(18) 0.45490(17) 0.34143(16) 0.0471(11) Uani 1 1 d G . . C26 C 0.5478(3) 0.39549(14) 0.32345(16) 0.0601(13) Uani 1 1 d G . . H26 H 0.5162 0.3514 0.3147 0.072 Uiso 1 1 calc R . . C27 C 0.6517(2) 0.40194(19) 0.31853(17) 0.0715(15) Uani 1 1 d G . . H27 H 0.6896 0.3622 0.3065 0.086 Uiso 1 1 calc R . . C28 C 0.69907(18) 0.4678(2) 0.33161(18) 0.0772(16) Uani 1 1 d G . . H28 H 0.7686 0.4721 0.3283 0.093 Uiso 1 1 calc R . . C29 C 0.6425(3) 0.52719(17) 0.34960(18) 0.0768(16) Uani 1 1 d G . . H29 H 0.6742 0.5712 0.3583 0.092 Uiso 1 1 calc R . . C30 C 0.5386(2) 0.52074(14) 0.35451(17) 0.0633(14) Uani 1 1 d G . . H30 H 0.5008 0.5605 0.3665 0.076 Uiso 1 1 calc R . . C31 C 0.3485(3) 0.37816(15) 0.41914(13) 0.0513(12) Uani 1 1 d G . . C32 C 0.4278(2) 0.37012(17) 0.47059(18) 0.0726(17) Uani 1 1 d G . . H32 H 0.4888 0.3938 0.4658 0.087 Uiso 1 1 calc R . . C33 C 0.4159(3) 0.3266(2) 0.52915(15) 0.097(2) Uani 1 1 d G . . H33 H 0.4690 0.3212 0.5636 0.116 Uiso 1 1 calc R . . C34 C 0.3247(4) 0.29115(18) 0.53626(15) 0.091(2) Uani 1 1 d G . . H34 H 0.3168 0.2620 0.5754 0.109 Uiso 1 1 calc R . . C35 C 0.2454(3) 0.29919(18) 0.4848(2) 0.0858(19) Uani 1 1 d G . . H35 H 0.1844 0.2755 0.4896 0.103 Uiso 1 1 calc R . . C36 C 0.2573(2) 0.34270(17) 0.42625(16) 0.0639(14) Uani 1 1 d G . . H36 H 0.2042 0.3481 0.3918 0.077 Uiso 1 1 calc R . . C37 C 0.0582(2) 0.52752(12) 0.21724(16) 0.0436(10) Uani 1 1 d G . . C38 C 0.1146(2) 0.57218(16) 0.17616(16) 0.0539(12) Uani 1 1 d G . . H38 H 0.1721 0.5546 0.1564 0.065 Uiso 1 1 calc R . . C39 C 0.0852(3) 0.64319(15) 0.16461(17) 0.0740(16) Uani 1 1 d G . . H39 H 0.1229 0.6731 0.1371 0.089 Uiso 1 1 calc R . . C40 C -0.0007(3) 0.66953(12) 0.1941(2) 0.0760(17) Uani 1 1 d G . . H40 H -0.0204 0.7170 0.1864 0.091 Uiso 1 1 calc R . . C41 C -0.0571(2) 0.62486(18) 0.23520(19) 0.0744(16) Uani 1 1 d G . . H41 H -0.1146 0.6425 0.2550 0.089 Uiso 1 1 calc R . . C42 C -0.0276(2) 0.55386(16) 0.24676(16) 0.0648(14) Uani 1 1 d G . . H42 H -0.0654 0.5240 0.2742 0.078 Uiso 1 1 calc R . . C43 C 0.0329(2) 0.40923(17) 0.30664(15) 0.0506(11) Uani 1 1 d G . . C44 C 0.0667(2) 0.44314(19) 0.36930(19) 0.0779(16) Uani 1 1 d G . . H44 H 0.1187 0.4768 0.3693 0.093 Uiso 1 1 calc R . . C45 C 0.0228(3) 0.4268(2) 0.43196(15) 0.103(2) Uani 1 1 d G . . H45 H 0.0454 0.4495 0.4739 0.124 Uiso 1 1 calc R . . C46 C -0.0549(3) 0.3765(2) 0.43195(19) 0.099(2) Uani 1 1 d G . . H46 H -0.0843 0.3655 0.4739 0.118 Uiso 1 1 calc R . . C47 C -0.0887(2) 0.34259(18) 0.3693(3) 0.093(2) Uani 1 1 d G . . H47 H -0.1407 0.3090 0.3693 0.111 Uiso 1 1 calc R . . C48 C -0.0448(2) 0.35895(17) 0.30663(19) 0.0643(14) Uani 1 1 d G . . H48 H -0.0674 0.3363 0.2647 0.077 Uiso 1 1 calc R . . C49 C 0.0259(2) 0.38888(15) 0.15402(14) 0.0450(11) Uani 1 1 d G . . C50 C -0.0361(2) 0.42676(13) 0.10482(16) 0.0532(12) Uani 1 1 d G . . H50 H -0.0460 0.4759 0.1106 0.064 Uiso 1 1 calc R . . C51 C -0.0833(2) 0.39126(19) 0.04695(15) 0.0681(15) Uani 1 1 d G . . H51 H -0.1248 0.4166 0.0140 0.082 Uiso 1 1 calc R . . C52 C -0.0685(3) 0.31788(19) 0.03828(16) 0.0728(16) Uani 1 1 d G . . H52 H -0.1001 0.2941 -0.0004 0.087 Uiso 1 1 calc R . . C53 C -0.0065(3) 0.28000(13) 0.0875(2) 0.0788(17) Uani 1 1 d G . . H53 H 0.0034 0.2309 0.0817 0.095 Uiso 1 1 calc R . . C54 C 0.0407(2) 0.31550(15) 0.14535(17) 0.0644(14) Uani 1 1 d G . . H54 H 0.0822 0.2902 0.1783 0.077 Uiso 1 1 calc R . . I1 I 0.29005(2) 0.265675(15) 0.244764(17) 0.05219(12) Uani 1 1 d . . . Cu2 Cu 0.27326(4) 0.40915(3) 0.23635(2) 0.03532(13) Uani 1 1 d . . . P3 P 0.36580(8) 0.44465(5) 0.14095(5) 0.0352(2) Uani 1 1 d . . . P4 P 0.09878(8) 0.43343(6) 0.22789(6) 0.0390(3) Uani 1 1 d . . . P5 P 0.35480(9) 0.44127(6) 0.34533(6) 0.0420(3) 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 0.035(2) 0.048(2) 0.033(2) 0.0037(18) 0.0081(17) -0.001(2) C2 0.046(3) 0.048(3) 0.047(3) 0.003(2) 0.008(2) 0.004(2) C3 0.060(3) 0.061(3) 0.051(3) 0.005(2) 0.009(2) 0.016(3) C4 0.044(3) 0.084(4) 0.051(3) 0.009(3) 0.009(2) 0.018(3) C5 0.041(3) 0.080(4) 0.064(3) 0.008(3) 0.010(2) 0.000(3) C6 0.046(3) 0.050(3) 0.054(3) 0.009(2) 0.006(2) 0.001(2) C7 0.043(2) 0.029(2) 0.037(2) 0.0021(16) 0.0066(18) -0.0065(18) C8 0.037(2) 0.057(3) 0.054(3) -0.005(2) 0.008(2) -0.002(2) C9 0.046(3) 0.088(4) 0.059(3) -0.005(3) -0.009(3) -0.012(3) C10 0.072(4) 0.071(3) 0.042(3) -0.007(2) -0.005(3) -0.013(3) C11 0.069(3) 0.061(3) 0.039(3) -0.004(2) 0.016(2) -0.005(3) C12 0.047(3) 0.053(3) 0.047(3) 0.001(2) 0.010(2) -0.004(2) C13 0.037(2) 0.042(2) 0.039(2) 0.0038(18) 0.0100(19) 0.0010(19) C14 0.050(3) 0.041(2) 0.043(3) 0.0036(19) 0.005(2) 0.001(2) C15 0.075(4) 0.046(3) 0.060(3) 0.017(2) 0.006(3) 0.002(3) C16 0.093(4) 0.037(3) 0.092(4) -0.001(3) 0.020(3) -0.003(3) C17 0.115(5) 0.054(3) 0.057(3) -0.014(3) 0.010(3) -0.015(3) C18 0.091(4) 0.046(3) 0.041(3) -0.004(2) 0.008(3) -0.009(3) C19 0.043(3) 0.042(2) 0.040(2) 0.0009(19) 0.004(2) -0.001(2) C20 0.065(3) 0.046(3) 0.045(3) 0.004(2) 0.005(2) -0.005(2) C21 0.066(3) 0.045(3) 0.066(3) 0.011(2) 0.002(3) 0.000(2) C22 0.067(4) 0.048(3) 0.075(4) -0.009(3) 0.021(3) 0.004(2) C23 0.086(4) 0.080(4) 0.051(3) -0.025(3) 0.002(3) 0.023(3) C24 0.068(3) 0.068(3) 0.043(3) -0.010(2) -0.004(2) 0.018(3) C25 0.052(3) 0.056(3) 0.032(2) -0.0016(19) -0.008(2) 0.008(2) C26 0.066(3) 0.070(3) 0.043(3) -0.003(2) -0.005(2) 0.011(3) C27 0.062(4) 0.099(4) 0.053(3) 0.000(3) 0.002(3) 0.018(3) C28 0.052(3) 0.118(5) 0.063(4) -0.003(3) 0.008(3) 0.001(4) C29 0.064(4) 0.087(4) 0.078(4) -0.007(3) -0.003(3) -0.012(3) C30 0.055(3) 0.067(3) 0.067(3) -0.014(3) -0.005(3) 0.004(3) C31 0.075(3) 0.039(2) 0.039(3) 0.0030(19) 0.005(2) 0.007(2) C32 0.111(5) 0.059(3) 0.045(3) 0.005(2) -0.020(3) 0.003(3) C33 0.174(8) 0.060(4) 0.052(4) 0.009(3) -0.026(4) 0.007(4) C34 0.183(8) 0.047(3) 0.044(3) 0.012(2) 0.012(4) 0.019(4) C35 0.129(6) 0.057(3) 0.077(4) 0.011(3) 0.049(4) 0.005(4) C36 0.092(4) 0.051(3) 0.050(3) 0.010(2) 0.017(3) 0.010(3) C37 0.041(3) 0.043(2) 0.047(3) -0.002(2) -0.002(2) 0.003(2) C38 0.060(3) 0.048(3) 0.053(3) 0.003(2) 0.003(2) 0.003(2) C39 0.095(5) 0.050(3) 0.076(4) 0.016(3) 0.000(3) 0.004(3) C40 0.094(5) 0.046(3) 0.084(4) -0.006(3) -0.018(4) 0.012(3) C41 0.070(4) 0.067(4) 0.086(4) -0.014(3) 0.003(3) 0.027(3) C42 0.056(3) 0.055(3) 0.085(4) 0.010(3) 0.017(3) 0.010(3) C43 0.042(3) 0.055(3) 0.056(3) 0.011(2) 0.013(2) 0.019(2) C44 0.070(4) 0.107(4) 0.059(4) -0.002(3) 0.020(3) -0.002(3) C45 0.099(5) 0.153(7) 0.062(4) -0.008(4) 0.037(4) 0.017(5) C46 0.092(5) 0.112(5) 0.099(6) 0.042(4) 0.054(4) 0.032(4) C47 0.067(4) 0.075(4) 0.142(7) 0.036(4) 0.046(4) 0.018(3) C48 0.055(3) 0.064(3) 0.076(4) 0.025(3) 0.022(3) 0.001(3) C49 0.031(2) 0.053(3) 0.052(3) 0.000(2) 0.004(2) -0.006(2) C50 0.040(3) 0.060(3) 0.059(3) 0.005(2) 0.002(2) -0.003(2) C51 0.051(3) 0.089(4) 0.062(3) 0.012(3) -0.006(3) -0.008(3) C52 0.059(3) 0.091(4) 0.066(4) -0.007(3) -0.010(3) -0.027(3) C53 0.077(4) 0.065(4) 0.092(5) -0.013(3) -0.011(4) -0.016(3) C54 0.059(3) 0.049(3) 0.083(4) 0.000(3) -0.013(3) -0.002(3) I1 0.0633(2) 0.03830(16) 0.0560(2) 0.00405(13) 0.01155(15) -0.00111(14) Cu2 0.0377(3) 0.0367(3) 0.0318(3) -0.0008(2) 0.0036(2) -0.0010(2) P3 0.0357(6) 0.0368(5) 0.0338(6) 0.0036(4) 0.0066(5) -0.0001(5) P4 0.0345(6) 0.0404(6) 0.0426(6) 0.0034(5) 0.0064(5) 0.0022(5) P5 0.0524(7) 0.0423(6) 0.0306(6) 0.0000(5) -0.0010(5) 0.0016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 P3 1.837(2) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C7 P3 1.839(2) . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C13 P3 1.850(2) . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C19 P5 1.840(2) . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C25 P5 1.831(3) . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 P5 1.831(2) . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C37 P4 1.837(2) . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C43 P4 1.834(3) . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C49 P4 1.840(2) . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? I1 Cu2 2.6813(6) . ? Cu2 P5 2.3390(11) . ? Cu2 P3 2.3459(11) . ? Cu2 P4 2.3480(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.0 . . ? C2 C1 P3 116.76(16) . . ? C6 C1 P3 123.18(16) . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 P3 117.72(16) . . ? C12 C7 P3 122.26(16) . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 P3 122.41(15) . . ? C18 C13 P3 117.56(15) . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 P5 117.21(16) . . ? C24 C19 P5 122.79(16) . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 P5 116.72(19) . . ? C30 C25 P5 123.28(19) . . ? C27 C26 C25 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C29 120.0 . . ? C30 C29 C28 120.0 . . ? C29 C30 C25 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 P5 122.11(19) . . ? C36 C31 P5 117.63(19) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C38 C37 C42 120.0 . . ? C38 C37 P4 117.80(18) . . ? C42 C37 P4 122.17(18) . . ? C37 C38 C39 120.0 . . ? C38 C39 C40 120.0 . . ? C41 C40 C39 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C37 120.0 . . ? C44 C43 C48 120.0 . . ? C44 C43 P4 116.0(2) . . ? C48 C43 P4 123.9(2) . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C43 120.0 . . ? C50 C49 C54 120.0 . . ? C50 C49 P4 122.37(17) . . ? C54 C49 P4 117.45(17) . . ? C49 C50 C51 120.0 . . ? C52 C51 C50 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C53 C54 C49 120.0 . . ? P5 Cu2 P3 111.92(4) . . ? P5 Cu2 P4 113.77(5) . . ? P3 Cu2 P4 117.18(4) . . ? P5 Cu2 I1 99.82(3) . . ? P3 Cu2 I1 106.28(3) . . ? P4 Cu2 I1 105.82(3) . . ? C1 P3 C7 101.33(13) . . ? C1 P3 C13 103.05(13) . . ? C7 P3 C13 101.98(13) . . ? C1 P3 Cu2 115.32(10) . . ? C7 P3 Cu2 117.26(10) . . ? C13 P3 Cu2 115.69(10) . . ? C43 P4 C37 99.86(15) . . ? C43 P4 C49 104.67(16) . . ? C37 P4 C49 102.22(14) . . ? C43 P4 Cu2 114.71(11) . . ? C37 P4 Cu2 117.98(10) . . ? C49 P4 Cu2 115.27(11) . . ? C25 P5 C31 102.51(15) . . ? C25 P5 C19 102.43(14) . . ? C31 P5 C19 103.33(14) . . ? C25 P5 Cu2 113.36(11) . . ? C31 P5 Cu2 117.82(11) . . ? C19 P5 Cu2 115.43(10) . . ? _diffrn_measured_fraction_theta_max 0.851 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.150 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.072