Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Gudat, Dietrich' ; Institut fur Anorganische Chemie Universitat Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; 'Nieger, Martin' ; Institut fur Anorganische Chemie Universitat Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; 'Schmitz, Katja' ; Institut fur Anorganische Chemie Universitat Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; 'Szarvas, Laslo' ; Institut fur Anorganische Chemie Universitat Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; _publ_contact_author_name 'Prof Dietrich Gudat' _publ_contact_author_address ; Institut fur Anorganische Chemie Universitat Bonn Gerhard-Domagk-Str. 1 Bonn 53121 GERMANY ; _publ_contact_author_phone '049 228 73-5823' _publ_contact_author_fax '049 228 73-5327' _publ_contact_author_email 'NIEGER@JOYX.JOENSUU.FI' _publ_requested_journal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; enclosed you will fond the necessary data for our publication in Chem. Commun. ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Unusual Properties of the First Copper Complex Containing a pi(eta2)- coordinated Phosphorus-Carbon Double Bond Moiety ; #============================================================================== data_gut48_nm _database_code_CSD 184981 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Bis-(1-triphenylphosphonio-benzo[c]phospholide) copper iodide] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H40 Cu I P4' _chemical_formula_sum 'C52 H40 Cu I P4' _chemical_formula_weight 979.16 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5944(2) _cell_length_b 11.4496(2) _cell_length_c 20.0383(15) _cell_angle_alpha 88.5390(10) _cell_angle_beta 78.5760(10) _cell_angle_gamma 64.676(2) _cell_volume 2148.75(17) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5082 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.412 _exptl_absorpt_correction_type 'empirical from multiple refl.' _exptl_absorpt_correction_T_min 0.6765 _exptl_absorpt_correction_T_max 0.8288 _exptl_absorpt_process_details 'MULABS (Platon; cf. Blessing, 1995)' _exptl_special_details ; dx = 40 mm; 180 sec./deg., 1 deg., 4 sets, 371 frames; mos.= 0.700(2) deg. ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 18029 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0696 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7328 _reflns_number_gt 5768 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7328 _refine_ls_number_parameters 529 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.17200(3) 0.62871(3) 0.436153(13) 0.02204(11) Uani 1 1 d . . . Cu1 Cu 0.34075(5) 0.55409(5) 0.32164(3) 0.02260(15) Uani 1 1 d . . . P1 P 0.51303(11) 0.64370(11) 0.28781(6) 0.0205(3) Uani 1 1 d . . . C2 C 0.5970(4) 0.5772(4) 0.2035(2) 0.0188(9) Uani 1 1 d . . . C3 C 0.5029(4) 0.6226(4) 0.1570(2) 0.0188(9) Uani 1 1 d . . . C4 C 0.5290(4) 0.5998(4) 0.0861(2) 0.0225(10) Uani 1 1 d . . . H4 H 0.6216 0.5422 0.0623 0.027 Uiso 1 1 calc R . . C5 C 0.4219(4) 0.6598(4) 0.0504(2) 0.0236(10) Uani 1 1 d . . . H5 H 0.4415 0.6445 0.0023 0.028 Uiso 1 1 calc R . . C6 C 0.2833(4) 0.7438(4) 0.0852(2) 0.0254(10) Uani 1 1 d . . . H6 H 0.2097 0.7841 0.0604 0.030 Uiso 1 1 calc R . . C7 C 0.2540(4) 0.7676(4) 0.1541(2) 0.0239(10) Uani 1 1 d . . . H7 H 0.1601 0.8248 0.1767 0.029 Uiso 1 1 calc R . . C8 C 0.3603(4) 0.7092(4) 0.1921(2) 0.0179(9) Uani 1 1 d . . . C9 C 0.3495(4) 0.7281(4) 0.2632(2) 0.0198(9) Uani 1 1 d D . . H9 H 0.267(3) 0.785(3) 0.2946(17) 0.024 Uiso 1 1 d D . . P2 P 0.78147(10) 0.48370(10) 0.18154(5) 0.0178(2) Uani 1 1 d . . . C10 C 0.8539(4) 0.4614(4) 0.2569(2) 0.0192(9) Uani 1 1 d . . . C11 C 0.9399(4) 0.5193(4) 0.2678(2) 0.0268(10) Uani 1 1 d . . . H11 H 0.9650 0.5701 0.2341 0.032 Uiso 1 1 calc R . . C12 C 0.9893(4) 0.5026(5) 0.3281(2) 0.0316(11) Uani 1 1 d . . . H12 H 1.0489 0.5416 0.3356 0.038 Uiso 1 1 calc R . . C13 C 0.9529(4) 0.4308(4) 0.3769(2) 0.0292(11) Uani 1 1 d . . . H13 H 0.9862 0.4212 0.4183 0.035 Uiso 1 1 calc R . . C14 C 0.8686(5) 0.3725(4) 0.3665(2) 0.0286(11) Uani 1 1 d . . . H14 H 0.8437 0.3229 0.4008 0.034 Uiso 1 1 calc R . . C15 C 0.8191(4) 0.3852(4) 0.3062(2) 0.0275(10) Uani 1 1 d . . . H15 H 0.7627 0.3429 0.2986 0.033 Uiso 1 1 calc R . . C16 C 0.8646(4) 0.5651(4) 0.1229(2) 0.0196(9) Uani 1 1 d . . . C17 C 0.7847(4) 0.6929(4) 0.1101(2) 0.0253(10) Uani 1 1 d . . . H17 H 0.6862 0.7348 0.1309 0.030 Uiso 1 1 calc R . . C18 C 0.8457(5) 0.7603(4) 0.0679(2) 0.0289(11) Uani 1 1 d . . . H18 H 0.7895 0.8471 0.0590 0.035 Uiso 1 1 calc R . . C19 C 0.9898(5) 0.6997(5) 0.0388(2) 0.0283(11) Uani 1 1 d . . . H19 H 1.0324 0.7449 0.0091 0.034 Uiso 1 1 calc R . . C20 C 1.0718(5) 0.5748(4) 0.0525(2) 0.0282(11) Uani 1 1 d . . . H20 H 1.1712 0.5352 0.0333 0.034 Uiso 1 1 calc R . . C21 C 1.0108(4) 0.5061(4) 0.0940(2) 0.0252(10) Uani 1 1 d . . . H21 H 1.0678 0.4193 0.1028 0.030 Uiso 1 1 calc R . . C22 C 0.8327(4) 0.3225(4) 0.1455(2) 0.0193(9) Uani 1 1 d . . . C23 C 0.9743(4) 0.2269(4) 0.1403(2) 0.0229(10) Uani 1 1 d . . . H23 H 1.0429 0.2473 0.1550 0.028 Uiso 1 1 calc R . . C24 C 1.0122(5) 0.1039(4) 0.1136(2) 0.0276(11) Uani 1 1 d . . . H24 H 1.1076 0.0399 0.1098 0.033 Uiso 1 1 calc R . . C25 C 0.9137(4) 0.0722(4) 0.0923(2) 0.0272(10) Uani 1 1 d . . . H25 H 0.9418 -0.0127 0.0734 0.033 Uiso 1 1 calc R . . C26 C 0.7730(5) 0.1648(4) 0.0987(2) 0.0262(10) Uani 1 1 d . . . H26 H 0.7047 0.1427 0.0849 0.031 Uiso 1 1 calc R . . C27 C 0.7326(4) 0.2897(4) 0.1252(2) 0.0229(10) Uani 1 1 d . . . H27 H 0.6368 0.3529 0.1294 0.027 Uiso 1 1 calc R . . P1' P 0.37327(11) 0.38747(11) 0.25445(6) 0.0208(3) Uani 1 1 d . . . C2' C 0.4083(4) 0.2245(4) 0.2608(2) 0.0201(9) Uani 1 1 d . . . C3' C 0.4017(4) 0.1704(4) 0.1986(2) 0.0193(9) Uani 1 1 d . . . C4' C 0.4225(4) 0.0438(4) 0.1813(2) 0.0250(10) Uani 1 1 d . . . H4' H 0.4446 -0.0200 0.2138 0.030 Uiso 1 1 calc R . . C5' C 0.4110(4) 0.0120(4) 0.1179(2) 0.0262(10) Uani 1 1 d . . . H5' H 0.4254 -0.0736 0.1069 0.031 Uiso 1 1 calc R . . C6' C 0.3782(4) 0.1048(5) 0.0690(2) 0.0286(11) Uani 1 1 d . . . H6' H 0.3700 0.0816 0.0254 0.034 Uiso 1 1 calc R . . C7' C 0.3581(4) 0.2285(4) 0.0836(2) 0.0250(10) Uani 1 1 d . . . H7' H 0.3369 0.2899 0.0499 0.030 Uiso 1 1 calc R . . C8' C 0.3685(4) 0.2660(4) 0.1482(2) 0.0201(9) Uani 1 1 d . . . C9' C 0.3496(4) 0.3884(4) 0.1727(2) 0.0213(10) Uani 1 1 d D . . H9' H 0.321(4) 0.464(3) 0.1474(19) 0.026 Uiso 1 1 d D . . P2' P 0.44724(11) 0.13658(10) 0.33248(5) 0.0183(2) Uani 1 1 d . . . C10' C 0.3289(4) 0.0611(4) 0.3583(2) 0.0208(9) Uani 1 1 d . . . C11' C 0.1986(4) 0.1090(4) 0.3371(2) 0.0279(11) Uani 1 1 d . . . H11' H 0.1780 0.1746 0.3056 0.033 Uiso 1 1 calc R . . C12' C 0.1002(4) 0.0614(4) 0.3619(3) 0.0295(11) Uani 1 1 d . . . H12' H 0.0129 0.0924 0.3465 0.035 Uiso 1 1 calc R . . C13' C 0.1289(5) -0.0319(4) 0.4095(2) 0.0310(11) Uani 1 1 d . . . H13' H 0.0592 -0.0618 0.4282 0.037 Uiso 1 1 calc R . . C14' C 0.2580(5) -0.0815(4) 0.4298(2) 0.0325(11) Uani 1 1 d . . . H14' H 0.2779 -0.1467 0.4616 0.039 Uiso 1 1 calc R . . C15' C 0.3581(4) -0.0364(4) 0.4038(2) 0.0250(10) Uani 1 1 d . . . H15' H 0.4478 -0.0721 0.4170 0.030 Uiso 1 1 calc R . . C16' C 0.4290(4) 0.2346(4) 0.4057(2) 0.0222(10) Uani 1 1 d . . . C17' C 0.3271(5) 0.2512(4) 0.4639(2) 0.0290(11) Uani 1 1 d . . . H17' H 0.2555 0.2222 0.4637 0.035 Uiso 1 1 calc R . . C18' C 0.3299(6) 0.3110(4) 0.5230(2) 0.0359(12) Uani 1 1 d . . . H18' H 0.2598 0.3225 0.5632 0.043 Uiso 1 1 calc R . . C19' C 0.4329(5) 0.3533(4) 0.5237(3) 0.0346(12) Uani 1 1 d . . . H19' H 0.4356 0.3917 0.5646 0.042 Uiso 1 1 calc R . . C20' C 0.5320(5) 0.3401(4) 0.4653(3) 0.0356(12) Uani 1 1 d . . . H20' H 0.6011 0.3722 0.4654 0.043 Uiso 1 1 calc R . . C21' C 0.5320(4) 0.2806(4) 0.4064(2) 0.0271(11) Uani 1 1 d . . . H21' H 0.6017 0.2707 0.3663 0.033 Uiso 1 1 calc R . . C22' C 0.6315(4) 0.0145(4) 0.3188(2) 0.0200(9) Uani 1 1 d . . . C23' C 0.6934(4) -0.0355(4) 0.3749(2) 0.0249(10) Uani 1 1 d . . . H23' H 0.6383 -0.0081 0.4200 0.030 Uiso 1 1 calc R . . C24' C 0.8351(4) -0.1248(4) 0.3647(2) 0.0276(11) Uani 1 1 d . . . H24' H 0.8773 -0.1598 0.4026 0.033 Uiso 1 1 calc R . . C25' C 0.9150(5) -0.1627(4) 0.2989(3) 0.0312(11) Uani 1 1 d . . . H25' H 1.0125 -0.2232 0.2920 0.037 Uiso 1 1 calc R . . C26' C 0.8559(4) -0.1147(5) 0.2439(2) 0.0315(11) Uani 1 1 d . . . H26' H 0.9120 -0.1427 0.1991 0.038 Uiso 1 1 calc R . . C27' C 0.7130(4) -0.0243(4) 0.2532(2) 0.0259(10) Uani 1 1 d . . . H27' H 0.6721 0.0102 0.2148 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.02212(16) 0.02434(18) 0.02008(18) 0.00406(12) -0.00620(12) -0.00978(13) Cu1 0.0217(3) 0.0246(3) 0.0227(3) 0.0021(2) -0.0047(2) -0.0111(2) P1 0.0200(5) 0.0223(6) 0.0190(6) 0.0008(5) -0.0044(5) -0.0088(5) C2 0.016(2) 0.020(2) 0.023(2) 0.0015(18) -0.0059(18) -0.0082(18) C3 0.017(2) 0.021(2) 0.021(2) 0.0039(18) -0.0047(18) -0.0107(18) C4 0.018(2) 0.026(3) 0.023(3) -0.0009(19) -0.0019(19) -0.0097(19) C5 0.025(2) 0.032(3) 0.019(2) 0.005(2) -0.011(2) -0.015(2) C6 0.021(2) 0.029(3) 0.031(3) 0.010(2) -0.013(2) -0.012(2) C7 0.016(2) 0.018(2) 0.036(3) 0.005(2) -0.006(2) -0.0057(18) C8 0.018(2) 0.015(2) 0.022(2) 0.0035(18) -0.0028(18) -0.0090(18) C9 0.017(2) 0.017(2) 0.022(2) -0.0013(18) 0.0016(18) -0.0059(18) P2 0.0146(5) 0.0213(6) 0.0177(6) 0.0030(5) -0.0046(4) -0.0074(5) C10 0.014(2) 0.022(2) 0.018(2) 0.0007(18) -0.0033(18) -0.0044(18) C11 0.023(2) 0.032(3) 0.027(3) 0.003(2) -0.008(2) -0.012(2) C12 0.023(2) 0.043(3) 0.032(3) -0.002(2) -0.011(2) -0.015(2) C13 0.023(2) 0.034(3) 0.022(3) 0.001(2) -0.007(2) -0.003(2) C14 0.027(2) 0.029(3) 0.023(3) 0.007(2) -0.003(2) -0.007(2) C15 0.026(2) 0.029(3) 0.029(3) 0.006(2) -0.008(2) -0.012(2) C16 0.022(2) 0.025(2) 0.019(2) 0.0046(18) -0.0081(19) -0.0147(19) C17 0.021(2) 0.027(3) 0.032(3) 0.005(2) -0.011(2) -0.012(2) C18 0.031(3) 0.032(3) 0.035(3) 0.011(2) -0.018(2) -0.019(2) C19 0.039(3) 0.042(3) 0.021(3) 0.010(2) -0.012(2) -0.030(2) C20 0.026(2) 0.037(3) 0.024(3) 0.002(2) 0.000(2) -0.018(2) C21 0.021(2) 0.027(3) 0.028(3) 0.002(2) -0.004(2) -0.011(2) C22 0.021(2) 0.019(2) 0.018(2) 0.0043(18) -0.0063(18) -0.0083(18) C23 0.020(2) 0.025(3) 0.026(3) 0.007(2) -0.0074(19) -0.0111(19) C24 0.023(2) 0.023(3) 0.031(3) 0.009(2) -0.005(2) -0.005(2) C25 0.031(2) 0.017(2) 0.027(3) 0.002(2) 0.001(2) -0.008(2) C26 0.028(2) 0.032(3) 0.023(3) 0.002(2) -0.004(2) -0.017(2) C27 0.020(2) 0.025(3) 0.020(2) 0.0035(19) -0.0038(19) -0.0059(19) P1' 0.0219(6) 0.0208(6) 0.0208(6) 0.0034(5) -0.0060(5) -0.0097(5) C2' 0.016(2) 0.024(2) 0.019(2) 0.0060(19) -0.0079(18) -0.0068(18) C3' 0.0133(19) 0.023(2) 0.020(2) 0.0036(18) -0.0048(18) -0.0065(18) C4' 0.022(2) 0.027(3) 0.026(3) 0.004(2) -0.008(2) -0.010(2) C5' 0.023(2) 0.024(3) 0.029(3) -0.005(2) -0.005(2) -0.008(2) C6' 0.022(2) 0.039(3) 0.021(3) -0.004(2) -0.008(2) -0.008(2) C7' 0.020(2) 0.031(3) 0.021(2) 0.005(2) -0.0081(19) -0.007(2) C8' 0.0123(19) 0.028(3) 0.018(2) 0.0036(19) -0.0024(18) -0.0075(18) C9' 0.018(2) 0.023(3) 0.022(2) 0.0062(19) -0.0050(19) -0.0085(19) P2' 0.0177(5) 0.0179(6) 0.0197(6) 0.0038(5) -0.0067(5) -0.0071(5) C10' 0.018(2) 0.017(2) 0.022(2) 0.0005(18) -0.0038(19) -0.0032(18) C11' 0.019(2) 0.024(3) 0.037(3) 0.009(2) -0.007(2) -0.006(2) C12' 0.018(2) 0.021(3) 0.049(3) 0.008(2) -0.011(2) -0.007(2) C13' 0.024(2) 0.027(3) 0.040(3) -0.002(2) 0.002(2) -0.012(2) C14' 0.041(3) 0.025(3) 0.035(3) 0.007(2) -0.011(2) -0.018(2) C15' 0.027(2) 0.021(2) 0.030(3) 0.006(2) -0.011(2) -0.011(2) C16' 0.025(2) 0.016(2) 0.022(3) 0.0045(18) -0.010(2) -0.0043(19) C17' 0.034(3) 0.020(2) 0.030(3) 0.006(2) -0.005(2) -0.010(2) C18' 0.051(3) 0.022(3) 0.019(3) 0.003(2) -0.001(2) -0.004(2) C19' 0.054(3) 0.020(3) 0.028(3) 0.002(2) -0.023(3) -0.008(2) C20' 0.034(3) 0.027(3) 0.045(3) -0.002(2) -0.023(3) -0.006(2) C21' 0.023(2) 0.024(3) 0.033(3) 0.003(2) -0.011(2) -0.007(2) C22' 0.018(2) 0.019(2) 0.025(3) 0.0029(19) -0.0065(19) -0.0094(18) C23' 0.022(2) 0.031(3) 0.026(3) 0.007(2) -0.007(2) -0.014(2) C24' 0.022(2) 0.026(3) 0.038(3) 0.013(2) -0.014(2) -0.011(2) C25' 0.016(2) 0.031(3) 0.045(3) 0.007(2) -0.008(2) -0.008(2) C26' 0.020(2) 0.039(3) 0.030(3) -0.001(2) 0.001(2) -0.009(2) C27' 0.021(2) 0.029(3) 0.029(3) 0.005(2) -0.008(2) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.5218(6) . ? Cu1 P1' 2.2262(12) . ? Cu1 C9 2.312(4) . ? Cu1 P1 2.4332(12) . ? P1 C9 1.749(4) . ? P1 C2 1.765(4) . ? C2 C3 1.426(5) . ? C2 P2 1.747(4) . ? C3 C4 1.402(6) . ? C3 C8 1.447(6) . ? C4 C5 1.378(5) . ? C4 H4 0.9500 . ? C5 C6 1.410(6) . ? C5 H5 0.9500 . ? C6 C7 1.361(6) . ? C6 H6 0.9500 . ? C7 C8 1.402(5) . ? C7 H7 0.9500 . ? C8 C9 1.421(6) . ? C9 H9 0.948(19) . ? P2 C10 1.791(4) . ? P2 C16 1.806(4) . ? P2 C22 1.811(4) . ? C10 C11 1.386(6) . ? C10 C15 1.400(6) . ? C11 C12 1.388(6) . ? C11 H11 0.9500 . ? C12 C13 1.363(7) . ? C12 H12 0.9500 . ? C13 C14 1.371(6) . ? C13 H13 0.9500 . ? C14 C15 1.389(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.390(6) . ? C16 C21 1.400(6) . ? C17 C18 1.380(6) . ? C17 H17 0.9500 . ? C18 C19 1.383(6) . ? C18 H18 0.9500 . ? C19 C20 1.374(6) . ? C19 H19 0.9500 . ? C20 C21 1.384(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.396(5) . ? C22 C23 1.414(5) . ? C23 C24 1.378(6) . ? C23 H23 0.9500 . ? C24 C25 1.383(6) . ? C24 H24 0.9500 . ? C25 C26 1.394(6) . ? C25 H25 0.9500 . ? C26 C27 1.391(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? P1' C9' 1.704(4) . ? P1' C2' 1.746(4) . ? C2' C3' 1.434(6) . ? C2' P2' 1.747(4) . ? C3' C4' 1.411(6) . ? C3' C8' 1.447(6) . ? C4' C5' 1.373(6) . ? C4' H4' 0.9500 . ? C5' C6' 1.405(6) . ? C5' H5' 0.9500 . ? C6' C7' 1.369(6) . ? C6' H6' 0.9500 . ? C7' C8' 1.413(6) . ? C7' H7' 0.9500 . ? C8' C9' 1.416(6) . ? C9' H9' 0.954(19) . ? P2' C10' 1.799(4) . ? P2' C16' 1.799(4) . ? P2' C22' 1.820(4) . ? C10' C15' 1.391(6) . ? C10' C11' 1.399(5) . ? C11' C12' 1.378(6) . ? C11' H11' 0.9500 . ? C12' C13' 1.389(6) . ? C12' H12' 0.9500 . ? C13' C14' 1.379(6) . ? C13' H13' 0.9500 . ? C14' C15' 1.379(6) . ? C14' H14' 0.9500 . ? C15' H15' 0.9500 . ? C16' C17' 1.378(6) . ? C16' C21' 1.401(6) . ? C17' C18' 1.395(7) . ? C17' H17' 0.9500 . ? C18' C19' 1.374(7) . ? C18' H18' 0.9500 . ? C19' C20' 1.372(7) . ? C19' H19' 0.9500 . ? C20' C21' 1.378(6) . ? C20' H20' 0.9500 . ? C21' H21' 0.9500 . ? C22' C27' 1.387(6) . ? C22' C23' 1.401(6) . ? C23' C24' 1.385(6) . ? C23' H23' 0.9500 . ? C24' C25' 1.384(7) . ? C24' H24' 0.9500 . ? C25' C26' 1.362(6) . ? C25' H25' 0.9500 . ? C26' C27' 1.399(6) . ? C26' H26' 0.9500 . ? C27' H27' 0.9500 . ? 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 P1' Cu1 C9 113.96(11) . . ? P1' Cu1 P1 115.00(4) . . ? C9 Cu1 P1 43.17(10) . . ? P1' Cu1 I1 125.47(4) . . ? C9 Cu1 I1 111.03(11) . . ? P1 Cu1 I1 118.68(3) . . ? C9 P1 C2 90.95(19) . . ? C9 P1 Cu1 64.73(14) . . ? C2 P1 Cu1 103.78(13) . . ? C3 C2 P2 125.8(3) . . ? C3 C2 P1 112.9(3) . . ? P2 C2 P1 120.8(2) . . ? C4 C3 C2 130.7(4) . . ? C4 C3 C8 118.5(3) . . ? C2 C3 C8 110.8(4) . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 120.6(4) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 121.0(4) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C7 C8 C9 128.1(4) . . ? C7 C8 C3 118.9(4) . . ? C9 C8 C3 112.9(3) . . ? C8 C9 P1 112.4(3) . . ? C8 C9 Cu1 111.7(3) . . ? P1 C9 Cu1 72.10(14) . . ? C8 C9 H9 126(2) . . ? P1 C9 H9 121(2) . . ? Cu1 C9 H9 90(3) . . ? C2 P2 C10 109.08(19) . . ? C2 P2 C16 110.53(19) . . ? C10 P2 C16 107.96(18) . . ? C2 P2 C22 113.80(19) . . ? C10 P2 C22 105.80(18) . . ? C16 P2 C22 109.4(2) . . ? C11 C10 C15 120.0(4) . . ? C11 C10 P2 121.8(3) . . ? C15 C10 P2 118.2(3) . . ? C10 C11 C12 119.5(4) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 120.6(4) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.3(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 120.7(4) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C10 118.8(4) . . ? C14 C15 H15 120.6 . . ? C10 C15 H15 120.6 . . ? C17 C16 C21 118.8(4) . . ? C17 C16 P2 119.5(3) . . ? C21 C16 P2 121.6(3) . . ? C18 C17 C16 121.3(4) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 119.2(4) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 120.5(4) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.6(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C16 119.7(4) . . ? C20 C21 H21 120.2 . . ? C16 C21 H21 120.2 . . ? C27 C22 C23 119.4(4) . . ? C27 C22 P2 120.8(3) . . ? C23 C22 P2 119.7(3) . . ? C24 C23 C22 119.5(4) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 121.1(4) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C24 C25 C26 119.9(4) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 119.9(4) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C22 120.2(4) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C9' P1' C2' 93.3(2) . . ? C9' P1' Cu1 128.04(16) . . ? C2' P1' Cu1 138.36(14) . . ? C3' C2' P1' 110.9(3) . . ? C3' C2' P2' 123.6(3) . . ? P1' C2' P2' 125.5(2) . . ? C4' C3' C2' 130.1(4) . . ? C4' C3' C8' 118.8(4) . . ? C2' C3' C8' 111.1(4) . . ? C5' C4' C3' 120.6(4) . . ? C5' C4' H4' 119.7 . . ? C3' C4' H4' 119.7 . . ? C4' C5' C6' 120.7(4) . . ? C4' C5' H5' 119.7 . . ? C6' C5' H5' 119.7 . . ? C7' C6' C5' 120.6(4) . . ? C7' C6' H6' 119.7 . . ? C5' C6' H6' 119.7 . . ? C6' C7' C8' 120.8(4) . . ? C6' C7' H7' 119.6 . . ? C8' C7' H7' 119.6 . . ? C7' C8' C9' 128.8(4) . . ? C7' C8' C3' 118.5(4) . . ? C9' C8' C3' 112.6(4) . . ? C8' C9' P1' 112.1(3) . . ? C8' C9' H9' 124(3) . . ? P1' C9' H9' 124(3) . . ? C2' P2' C10' 110.98(18) . . ? C2' P2' C16' 113.4(2) . . ? C10' P2' C16' 106.2(2) . . ? C2' P2' C22' 112.55(19) . . ? C10' P2' C22' 109.59(18) . . ? C16' P2' C22' 103.77(18) . . ? C15' C10' C11' 119.1(4) . . ? C15' C10' P2' 121.4(3) . . ? C11' C10' P2' 119.3(3) . . ? C12' C11' C10' 120.2(4) . . ? C12' C11' H11' 119.9 . . ? C10' C11' H11' 119.9 . . ? C11' C12' C13' 119.8(4) . . ? C11' C12' H12' 120.1 . . ? C13' C12' H12' 120.1 . . ? C14' C13' C12' 120.4(4) . . ? C14' C13' H13' 119.8 . . ? C12' C13' H13' 119.8 . . ? C15' C14' C13' 119.9(4) . . ? C15' C14' H14' 120.1 . . ? C13' C14' H14' 120.1 . . ? C14' C15' C10' 120.5(4) . . ? C14' C15' H15' 119.7 . . ? C10' C15' H15' 119.7 . . ? C17' C16' C21' 119.5(4) . . ? C17' C16' P2' 121.1(3) . . ? C21' C16' P2' 118.9(3) . . ? C16' C17' C18' 119.4(4) . . ? C16' C17' H17' 120.3 . . ? C18' C17' H17' 120.3 . . ? C19' C18' C17' 120.7(5) . . ? C19' C18' H18' 119.7 . . ? C17' C18' H18' 119.7 . . ? C20' C19' C18' 119.8(4) . . ? C20' C19' H19' 120.1 . . ? C18' C19' H19' 120.1 . . ? C19' C20' C21' 120.5(5) . . ? C19' C20' H20' 119.8 . . ? C21' C20' H20' 119.8 . . ? C20' C21' C16' 120.0(5) . . ? C20' C21' H21' 120.0 . . ? C16' C21' H21' 120.0 . . ? C27' C22' C23' 119.9(4) . . ? C27' C22' P2' 120.4(3) . . ? C23' C22' P2' 119.7(3) . . ? C24' C23' C22' 119.9(4) . . ? C24' C23' H23' 120.1 . . ? C22' C23' H23' 120.1 . . ? C25' C24' C23' 119.6(4) . . ? C25' C24' H24' 120.2 . . ? C23' C24' H24' 120.2 . . ? C26' C25' C24' 121.0(4) . . ? C26' C25' H25' 119.5 . . ? C24' C25' H25' 119.5 . . ? C25' C26' C27' 120.3(4) . . ? C25' C26' H26' 119.9 . . ? C27' C26' H26' 119.9 . . ? C22' C27' C26' 119.4(4) . . ? C22' C27' H27' 120.3 . . ? C26' C27' H27' 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1' Cu1 P1 C9 99.09(16) . . . . ? I1 Cu1 P1 C9 -90.84(16) . . . . ? P1' Cu1 P1 C2 14.64(14) . . . . ? C9 Cu1 P1 C2 -84.4(2) . . . . ? I1 Cu1 P1 C2 -175.29(13) . . . . ? C9 P1 C2 C3 2.2(3) . . . . ? Cu1 P1 C2 C3 66.4(3) . . . . ? C9 P1 C2 P2 174.3(3) . . . . ? Cu1 P1 C2 P2 -121.5(2) . . . . ? P2 C2 C3 C4 4.2(7) . . . . ? P1 C2 C3 C4 175.8(4) . . . . ? P2 C2 C3 C8 -173.5(3) . . . . ? P1 C2 C3 C8 -1.9(4) . . . . ? C2 C3 C4 C5 -176.6(4) . . . . ? C8 C3 C4 C5 1.0(6) . . . . ? C3 C4 C5 C6 -1.1(6) . . . . ? C4 C5 C6 C7 0.7(6) . . . . ? C5 C6 C7 C8 -0.2(6) . . . . ? C6 C7 C8 C9 176.7(4) . . . . ? C6 C7 C8 C3 0.2(6) . . . . ? C4 C3 C8 C7 -0.5(6) . . . . ? C2 C3 C8 C7 177.5(4) . . . . ? C4 C3 C8 C9 -177.6(4) . . . . ? C2 C3 C8 C9 0.5(5) . . . . ? C7 C8 C9 P1 -175.6(3) . . . . ? C3 C8 C9 P1 1.2(4) . . . . ? C7 C8 C9 Cu1 105.6(4) . . . . ? C3 C8 C9 Cu1 -77.7(4) . . . . ? C2 P1 C9 C8 -1.9(3) . . . . ? Cu1 P1 C9 C8 -106.7(3) . . . . ? C2 P1 C9 Cu1 104.81(15) . . . . ? P1' Cu1 C9 C8 6.0(3) . . . . ? P1 Cu1 C9 C8 107.6(3) . . . . ? I1 Cu1 C9 C8 -142.4(2) . . . . ? P1' Cu1 C9 P1 -101.66(12) . . . . ? I1 Cu1 C9 P1 109.98(11) . . . . ? C3 C2 P2 C10 175.7(3) . . . . ? P1 C2 P2 C10 4.7(3) . . . . ? C3 C2 P2 C16 57.2(4) . . . . ? P1 C2 P2 C16 -113.8(3) . . . . ? C3 C2 P2 C22 -66.4(4) . . . . ? P1 C2 P2 C22 122.6(2) . . . . ? C2 P2 C10 C11 -110.7(4) . . . . ? C16 P2 C10 C11 9.5(4) . . . . ? C22 P2 C10 C11 126.5(4) . . . . ? C2 P2 C10 C15 68.0(4) . . . . ? C16 P2 C10 C15 -171.8(3) . . . . ? C22 P2 C10 C15 -54.8(4) . . . . ? C15 C10 C11 C12 -0.9(6) . . . . ? P2 C10 C11 C12 177.7(3) . . . . ? C10 C11 C12 C13 -0.5(7) . . . . ? C11 C12 C13 C14 0.9(7) . . . . ? C12 C13 C14 C15 0.2(7) . . . . ? C13 C14 C15 C10 -1.6(7) . . . . ? C11 C10 C15 C14 2.0(6) . . . . ? P2 C10 C15 C14 -176.7(3) . . . . ? C2 P2 C16 C17 9.6(4) . . . . ? C10 P2 C16 C17 -109.7(3) . . . . ? C22 P2 C16 C17 135.7(3) . . . . ? C2 P2 C16 C21 -175.5(3) . . . . ? C10 P2 C16 C21 65.2(4) . . . . ? C22 P2 C16 C21 -49.5(4) . . . . ? C21 C16 C17 C18 2.2(6) . . . . ? P2 C16 C17 C18 177.2(3) . . . . ? C16 C17 C18 C19 -1.1(6) . . . . ? C17 C18 C19 C20 -1.0(6) . . . . ? C18 C19 C20 C21 2.0(7) . . . . ? C19 C20 C21 C16 -0.8(7) . . . . ? C17 C16 C21 C20 -1.2(6) . . . . ? P2 C16 C21 C20 -176.2(3) . . . . ? C2 P2 C22 C27 12.3(4) . . . . ? C10 P2 C22 C27 132.0(3) . . . . ? C16 P2 C22 C27 -111.9(3) . . . . ? C2 P2 C22 C23 -165.2(3) . . . . ? C10 P2 C22 C23 -45.5(4) . . . . ? C16 P2 C22 C23 70.6(4) . . . . ? C27 C22 C23 C24 1.6(6) . . . . ? P2 C22 C23 C24 179.1(3) . . . . ? C22 C23 C24 C25 -0.4(6) . . . . ? C23 C24 C25 C26 -1.0(6) . . . . ? C24 C25 C26 C27 1.3(6) . . . . ? C25 C26 C27 C22 -0.1(6) . . . . ? C23 C22 C27 C26 -1.4(6) . . . . ? P2 C22 C27 C26 -178.8(3) . . . . ? C9 Cu1 P1' C9' -21.7(2) . . . . ? P1 Cu1 P1' C9' -69.41(18) . . . . ? I1 Cu1 P1' C9' 121.29(18) . . . . ? C9 Cu1 P1' C2' 166.8(2) . . . . ? P1 Cu1 P1' C2' 119.1(2) . . . . ? I1 Cu1 P1' C2' -50.2(2) . . . . ? C9' P1' C2' C3' 0.1(3) . . . . ? Cu1 P1' C2' C3' 173.42(19) . . . . ? C9' P1' C2' P2' 179.8(3) . . . . ? Cu1 P1' C2' P2' -6.9(4) . . . . ? P1' C2' C3' C4' -180.0(3) . . . . ? P2' C2' C3' C4' 0.3(6) . . . . ? P1' C2' C3' C8' 0.2(4) . . . . ? P2' C2' C3' C8' -179.5(3) . . . . ? C2' C3' C4' C5' -180.0(4) . . . . ? C8' C3' C4' C5' -0.2(6) . . . . ? C3' C4' C5' C6' -0.1(6) . . . . ? C4' C5' C6' C7' 0.5(6) . . . . ? C5' C6' C7' C8' -0.6(6) . . . . ? C6' C7' C8' C9' -179.2(4) . . . . ? C6' C7' C8' C3' 0.3(6) . . . . ? C4' C3' C8' C7' 0.0(6) . . . . ? C2' C3' C8' C7' 179.9(3) . . . . ? C4' C3' C8' C9' 179.6(3) . . . . ? C2' C3' C8' C9' -0.5(5) . . . . ? C7' C8' C9' P1' -179.9(3) . . . . ? C3' C8' C9' P1' 0.6(4) . . . . ? C2' P1' C9' C8' -0.4(3) . . . . ? Cu1 P1' C9' C8' -174.8(2) . . . . ? C3' C2' P2' C10' -54.3(4) . . . . ? P1' C2' P2' C10' 126.0(3) . . . . ? C3' C2' P2' C16' -173.7(3) . . . . ? P1' C2' P2' C16' 6.6(3) . . . . ? C3' C2' P2' C22' 68.9(4) . . . . ? P1' C2' P2' C22' -110.8(3) . . . . ? C2' P2' C10' C15' 165.4(4) . . . . ? C16' P2' C10' C15' -71.0(4) . . . . ? C22' P2' C10' C15' 40.4(4) . . . . ? C2' P2' C10' C11' -20.4(4) . . . . ? C16' P2' C10' C11' 103.2(4) . . . . ? C22' P2' C10' C11' -145.3(3) . . . . ? C15' C10' C11' C12' 1.0(7) . . . . ? P2' C10' C11' C12' -173.4(4) . . . . ? C10' C11' C12' C13' 1.8(7) . . . . ? C11' C12' C13' C14' -3.0(7) . . . . ? C12' C13' C14' C15' 1.3(7) . . . . ? C13' C14' C15' C10' 1.5(7) . . . . ? C11' C10' C15' C14' -2.6(7) . . . . ? P2' C10' C15' C14' 171.6(4) . . . . ? C2' P2' C16' C17' 115.3(3) . . . . ? C10' P2' C16' C17' -6.8(4) . . . . ? C22' P2' C16' C17' -122.3(3) . . . . ? C2' P2' C16' C21' -73.0(4) . . . . ? C10' P2' C16' C21' 164.9(3) . . . . ? C22' P2' C16' C21' 49.4(4) . . . . ? C21' C16' C17' C18' -1.4(6) . . . . ? P2' C16' C17' C18' 170.3(3) . . . . ? C16' C17' C18' C19' 0.0(6) . . . . ? C17' C18' C19' C20' 1.8(7) . . . . ? C18' C19' C20' C21' -2.2(6) . . . . ? C19' C20' C21' C16' 0.9(6) . . . . ? C17' C16' C21' C20' 1.0(6) . . . . ? P2' C16' C21' C20' -170.9(3) . . . . ? C2' P2' C22' C27' -16.8(4) . . . . ? C10' P2' C22' C27' 107.2(3) . . . . ? C16' P2' C22' C27' -139.7(3) . . . . ? C2' P2' C22' C23' 159.8(3) . . . . ? C10' P2' C22' C23' -76.2(4) . . . . ? C16' P2' C22' C23' 36.9(4) . . . . ? C27' C22' C23' C24' -1.0(6) . . . . ? P2' C22' C23' C24' -177.6(3) . . . . ? C22' C23' C24' C25' 0.9(6) . . . . ? C23' C24' C25' C26' -0.8(7) . . . . ? C24' C25' C26' C27' 0.8(7) . . . . ? C23' C22' C27' C26' 1.0(6) . . . . ? P2' C22' C27' C26' 177.6(3) . . . . ? C25' C26' C27' C22' -1.0(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C13 H13 I1 0.95 3.23 3.864(5) 125.7 2_666 C12 H12 I1 0.95 3.00 3.838(4) 147.5 1_655 C12 H12 Cu1 0.95 3.11 3.989(4) 154.0 1_655 C13' H13' I1 0.95 3.23 3.750(5) 116.4 1_545 C24' H24' I1 0.95 3.22 3.994(4) 140.4 1_645 _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.421 _refine_diff_density_min -1.207 _refine_diff_density_rms 0.117 #============================================================================== _eof # End of Crystallographic Information File