# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Hakuba Kitagawa' 'Yoshiki Ozawa' 'Koshiro Toriumi' _publ_contact_author_name 'Yoshiki Ozawa' _publ_contact_author_email ozawa@sci.u-hyogo.ac.jp _publ_section_title ; Flexibility of cubane-like Cu4I4 framework: Temperature dependence of molecular structure and luminescence thermochromism of [Cu4I4(PPh3)4] in two polymorphic crystalline state ; # Attachment 'cubic-combined.cif.txt' data_cuipph_cubic_300k _database_code_depnum_ccdc_archive 'CCDC 777561' #TrackingRef 'cubic-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method toluene/ether _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colorless _diffrn_ambient_temperature 300(1) _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 0.0021 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 0.2614 1.2674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7268 1.8135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0905 0.0944 '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' _symmetry_space_group_name_hall 'I -4bd 2c 3' _symmetry_int_tables_number 220 _chemical_absolute_configuration ad 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 30.1826(5) _cell_length_b 30.1826(5) _cell_length_c 30.1826(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 27496.0(8) _cell_formula_units_Z 16 _cell_measurement_temperature 300(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14080 _exptl_absorpt_coefficient_mu 3.151 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6761 _exptl_absorpt_correction_T_max 0.7649 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal-focus sealed tube' _diffrn_source_type 'Rigaku R-AXIS' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID-F' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 112088 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 29.97 _reflns_number_total 6669 _reflns_number_gt 4198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_cell_refinement 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2006), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.1036P)^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 0.00(4) _refine_ls_number_reflns 6669 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1679 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 I2 I 0.992203(18) 0.037608(17) 0.922106(17) 0.05968(16) Uani 1 1 d . . . I1 I 1.054028(17) 0.054028(17) 1.054028(17) 0.0634(2) Uani 1 3 d S . . Cu1 Cu 0.96298(3) -0.03702(3) 0.96298(3) 0.0686(4) Uani 1 3 d S . . Cu2 Cu 1.05545(4) 0.01162(4) 0.97584(4) 0.0718(3) Uani 1 1 d . . . P1 P 0.91938(7) -0.08062(7) 0.91938(7) 0.0578(7) Uani 1 3 d S . . P2 P 1.12659(7) 0.00810(7) 0.95323(7) 0.0582(5) Uani 1 1 d . . . C12 C 1.1748(3) 0.0059(4) 1.0320(3) 0.075(2) Uani 1 1 d . . . H12 H 1.1697 0.0362 1.0334 0.090 Uiso 1 1 calc R . . C13 C 1.1565(3) 0.0593(3) 0.9419(3) 0.0620(18) Uani 1 1 d . . . C19 C 0.8600(3) -0.0696(3) 0.9242(3) 0.0606(18) Uani 1 1 d . . . C24 C 0.8282(3) -0.1016(3) 0.9171(3) 0.069(2) Uani 1 1 d . . . H24 H 0.8368 -0.1300 0.9090 0.083 Uiso 1 1 calc R . . C1 C 1.1386(3) -0.0238(3) 0.9031(3) 0.0627(19) Uani 1 1 d . . . C20 C 0.8464(3) -0.0276(3) 0.9358(4) 0.078(3) Uani 1 1 d . . . H20 H 0.8675 -0.0055 0.9403 0.094 Uiso 1 1 calc R . . C18 C 1.1325(4) 0.0952(3) 0.9265(3) 0.076(2) Uani 1 1 d . . . H18 H 1.1018 0.0946 0.9253 0.092 Uiso 1 1 calc R . . C7 C 1.1598(3) -0.0181(3) 0.9954(3) 0.0607(18) Uani 1 1 d . . . C5 C 1.1885(5) -0.0536(6) 0.8487(5) 0.134(6) Uani 1 1 d . . . H5 H 1.2174 -0.0579 0.8391 0.161 Uiso 1 1 calc R . . C14 C 1.2023(3) 0.0625(4) 0.9452(4) 0.087(3) Uani 1 1 d . . . H14 H 1.2182 0.0392 0.9574 0.105 Uiso 1 1 calc R . . C3 C 1.1121(5) -0.0592(4) 0.8375(4) 0.101(4) Uani 1 1 d . . . H3 H 1.0885 -0.0686 0.8201 0.121 Uiso 1 1 calc R . . C11 C 1.1969(4) -0.0148(5) 1.0661(3) 0.094(3) Uani 1 1 d . . . H11 H 1.2066 0.0015 1.0903 0.113 Uiso 1 1 calc R . . C10 C 1.2048(4) -0.0599(5) 1.0643(4) 0.101(4) Uani 1 1 d . . . H10 H 1.2209 -0.0736 1.0866 0.121 Uiso 1 1 calc R . . C21 C 0.8024(4) -0.0179(4) 0.9409(4) 0.093(3) Uani 1 1 d . . . H21 H 0.7937 0.0107 0.9486 0.111 Uiso 1 1 calc R . . C2 C 1.1039(3) -0.0376(3) 0.8767(3) 0.077(2) Uani 1 1 d . . . H2 H 1.0749 -0.0322 0.8855 0.093 Uiso 1 1 calc R . . C4 C 1.1549(5) -0.0671(4) 0.8234(4) 0.102(4) Uani 1 1 d . . . H4 H 1.1602 -0.0816 0.7967 0.123 Uiso 1 1 calc R . . C23 C 0.7829(3) -0.0916(4) 0.9221(4) 0.080(3) Uani 1 1 d . . . H23 H 0.7614 -0.1131 0.9168 0.096 Uiso 1 1 calc R . . C22 C 0.7709(3) -0.0501(4) 0.9348(4) 0.089(3) Uani 1 1 d . . . H22 H 0.7411 -0.0435 0.9394 0.107 Uiso 1 1 calc R . . C9 C 1.1890(4) -0.0840(4) 1.0298(5) 0.104(4) Uani 1 1 d . . . H9 H 1.1935 -0.1145 1.0293 0.124 Uiso 1 1 calc R . . C15 C 1.2243(4) 0.0993(5) 0.9309(5) 0.108(4) Uani 1 1 d . . . H15 H 1.2551 0.1002 0.9321 0.130 Uiso 1 1 calc R . . C17 C 1.1570(6) 0.1336(4) 0.9124(4) 0.101(4) Uani 1 1 d . . . H17 H 1.1419 0.1581 0.9014 0.121 Uiso 1 1 calc R . . C8 C 1.1663(4) -0.0641(3) 0.9957(4) 0.083(3) Uani 1 1 d . . . H8 H 1.1553 -0.0813 0.9727 0.100 Uiso 1 1 calc R . . C6 C 1.1809(4) -0.0331(6) 0.8899(5) 0.133(6) Uani 1 1 d . . . H6 H 1.2046 -0.0258 0.9082 0.160 Uiso 1 1 calc R . . C16 C 1.2015(5) 0.1344(4) 0.9151(4) 0.102(4) Uani 1 1 d . . . H16 H 1.2168 0.1595 0.9058 0.122 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 I2 0.0612(3) 0.0601(3) 0.0578(3) 0.0031(2) -0.0040(2) -0.0003(2) I1 0.0634(2) 0.0634(2) 0.0634(2) -0.0053(2) -0.0053(2) -0.0053(2) Cu1 0.0686(4) 0.0686(4) 0.0686(4) -0.0072(4) -0.0072(4) -0.0072(4) Cu2 0.0541(5) 0.0916(8) 0.0698(6) -0.0002(6) 0.0016(5) 0.0032(5) P1 0.0578(7) 0.0578(7) 0.0578(7) -0.0036(8) -0.0036(8) -0.0036(8) P2 0.0492(9) 0.0669(12) 0.0586(11) -0.0039(9) 0.0018(8) 0.0002(8) C12 0.067(5) 0.092(6) 0.066(5) -0.013(5) -0.004(4) 0.001(5) C13 0.068(5) 0.065(5) 0.054(4) -0.003(4) 0.008(3) -0.001(4) C19 0.070(5) 0.063(5) 0.049(4) -0.001(3) -0.002(3) -0.003(4) C24 0.067(5) 0.062(5) 0.077(6) -0.008(4) -0.001(4) -0.005(4) C1 0.064(5) 0.059(4) 0.065(5) -0.004(3) -0.007(4) -0.002(4) C20 0.061(5) 0.066(5) 0.106(8) -0.019(5) -0.014(5) 0.005(4) C18 0.089(6) 0.069(5) 0.072(6) -0.014(4) 0.002(5) 0.005(5) C7 0.046(4) 0.075(5) 0.061(4) -0.001(4) 0.006(3) 0.003(3) C5 0.116(10) 0.175(16) 0.112(9) -0.078(10) 0.040(8) -0.031(10) C14 0.061(5) 0.084(6) 0.118(8) 0.002(6) 0.014(5) -0.010(5) C3 0.125(10) 0.090(8) 0.088(8) -0.029(6) -0.035(7) -0.002(7) C11 0.083(7) 0.141(11) 0.059(5) -0.020(6) -0.008(5) 0.023(7) C10 0.071(6) 0.152(12) 0.081(7) 0.024(8) -0.005(5) 0.022(7) C21 0.076(6) 0.089(7) 0.113(8) -0.019(6) -0.010(6) 0.014(5) C2 0.080(6) 0.075(6) 0.077(6) -0.015(5) -0.023(5) 0.005(5) C4 0.147(12) 0.085(7) 0.075(7) -0.018(6) 0.006(7) 0.005(8) C23 0.051(4) 0.091(7) 0.097(7) 0.013(5) -0.006(4) -0.007(4) C22 0.064(6) 0.110(8) 0.092(7) -0.001(6) -0.004(5) 0.009(5) C9 0.100(9) 0.095(8) 0.116(10) 0.024(7) -0.025(7) 0.019(7) C15 0.076(7) 0.101(9) 0.148(12) 0.000(8) 0.015(7) -0.022(6) C17 0.156(13) 0.063(6) 0.083(7) 0.009(5) 0.012(8) 0.000(7) C8 0.086(6) 0.079(6) 0.084(6) -0.013(5) -0.017(5) 0.024(5) C6 0.068(6) 0.215(17) 0.116(10) -0.092(11) 0.022(6) -0.018(8) C16 0.129(11) 0.080(7) 0.097(8) 0.000(6) 0.029(7) -0.040(7) _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 I2 Cu2 2.6249(13) . ? I2 Cu1 2.7155(9) . ? I2 Cu2 2.7987(14) 17_546 ? I2 I2 4.3021(9) 9_645 ? I2 I1 4.4252(9) . ? I1 Cu2 2.6850(14) . ? I1 Cu2 2.6850(14) 17_546 ? I1 Cu2 2.6850(14) 9_645 ? Cu1 P1 2.279(4) . ? Cu1 I2 2.7155(9) 17_546 ? Cu1 I2 2.7155(9) 9_645 ? Cu1 Cu2 3.1775(19) . ? Cu2 P2 2.255(2) . ? Cu2 I2 2.7987(14) 9_645 ? Cu2 Cu2 2.9478(19) 17_546 ? Cu2 Cu2 2.9478(19) 9_645 ? P1 C19 1.829(9) 9_645 ? P1 C19 1.829(9) . ? P1 C19 1.829(9) 17_546 ? P2 C7 1.804(9) . ? P2 C13 1.822(9) . ? P2 C1 1.829(9) . ? C12 C11 1.376(15) . ? C12 C7 1.397(13) . ? C13 C18 1.384(13) . ? C13 C14 1.388(13) . ? C19 C24 1.377(12) . ? C19 C20 1.379(12) . ? C24 C23 1.410(13) . ? C1 C6 1.365(15) . ? C1 C2 1.381(12) . ? C20 C21 1.371(15) . ? C18 C17 1.436(17) . ? C7 C8 1.402(13) . ? C5 C4 1.333(19) . ? C5 C6 1.409(16) . ? C14 C15 1.365(17) . ? C3 C2 1.375(17) . ? C3 C4 1.38(2) . ? C11 C10 1.380(18) . ? C10 C9 1.357(19) . ? C21 C22 1.372(16) . ? C23 C22 1.359(16) . ? C9 C8 1.372(15) . ? C15 C16 1.35(2) . ? C17 C16 1.35(2) . ? 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 Cu2 I2 Cu1 73.00(4) . . ? Cu2 I2 Cu2 65.75(5) . 17_546 ? Cu1 I2 Cu2 70.35(4) . 17_546 ? Cu2 I2 I2 38.95(3) . 9_645 ? Cu1 I2 I2 37.62(2) . 9_645 ? Cu2 I2 I2 74.77(2) 17_546 9_645 ? Cu2 I2 I1 33.98(3) . . ? Cu1 I2 I1 79.70(4) . . ? Cu2 I2 I1 35.34(3) 17_546 . ? I2 I2 I1 60.916(8) 9_645 . ? Cu2 I1 Cu2 66.59(4) . 17_546 ? Cu2 I1 Cu2 66.59(4) . 9_645 ? Cu2 I1 Cu2 66.59(4) 17_546 9_645 ? Cu2 I1 I2 33.13(3) . . ? Cu2 I1 I2 37.08(3) 17_546 . ? Cu2 I1 I2 73.44(3) 9_645 . ? P1 Cu1 I2 113.84(4) . . ? P1 Cu1 I2 113.84(4) . 17_546 ? I2 Cu1 I2 104.77(4) . 17_546 ? P1 Cu1 I2 113.84(4) . 9_645 ? I2 Cu1 I2 104.77(4) . 9_645 ? I2 Cu1 I2 104.77(4) 17_546 9_645 ? P1 Cu1 Cu2 147.61(3) . . ? I2 Cu1 Cu2 52.19(3) . . ? I2 Cu1 Cu2 98.48(6) 17_546 . ? I2 Cu1 Cu2 56.05(4) 9_645 . ? P2 Cu2 I2 121.29(7) . . ? P2 Cu2 I1 107.68(7) . . ? I2 Cu2 I1 112.89(5) . . ? P2 Cu2 I2 101.02(7) . 9_645 ? I2 Cu2 I2 104.93(5) . 9_645 ? I1 Cu2 I2 107.58(4) . 9_645 ? P2 Cu2 Cu2 155.22(8) . 17_546 ? I2 Cu2 Cu2 59.96(4) . 17_546 ? I1 Cu2 Cu2 56.71(2) . 17_546 ? I2 Cu2 Cu2 102.23(3) 9_645 17_546 ? P2 Cu2 Cu2 131.04(9) . 9_645 ? I2 Cu2 Cu2 106.66(4) . 9_645 ? I1 Cu2 Cu2 56.71(2) . 9_645 ? I2 Cu2 Cu2 54.28(4) 9_645 9_645 ? Cu2 Cu2 Cu2 60.0 17_546 9_645 ? P2 Cu2 Cu1 141.03(8) . . ? I2 Cu2 Cu1 54.81(2) . . ? I1 Cu2 Cu1 108.28(4) . . ? I2 Cu2 Cu1 53.60(2) 9_645 . ? Cu2 Cu2 Cu1 62.36(2) 17_546 . ? Cu2 Cu2 Cu1 62.36(2) 9_645 . ? C19 P1 C19 103.9(3) 9_645 . ? C19 P1 C19 103.9(3) 9_645 17_546 ? C19 P1 C19 103.9(3) . 17_546 ? C19 P1 Cu1 114.6(3) 9_645 . ? C19 P1 Cu1 114.6(3) . . ? C19 P1 Cu1 114.6(3) 17_546 . ? C7 P2 C13 103.3(4) . . ? C7 P2 C1 104.0(4) . . ? C13 P2 C1 101.1(4) . . ? C7 P2 Cu2 109.6(3) . . ? C13 P2 Cu2 119.2(3) . . ? C1 P2 Cu2 117.7(3) . . ? C11 C12 C7 120.8(10) . . ? C18 C13 C14 119.3(9) . . ? C18 C13 P2 118.0(7) . . ? C14 C13 P2 122.6(7) . . ? C24 C19 C20 118.5(9) . . ? C24 C19 P1 122.9(7) . . ? C20 C19 P1 118.6(7) . . ? C19 C24 C23 120.6(9) . . ? C6 C1 C2 118.6(9) . . ? C6 C1 P2 122.3(7) . . ? C2 C1 P2 119.0(7) . . ? C21 C20 C19 120.9(10) . . ? C13 C18 C17 117.6(11) . . ? C12 C7 C8 117.6(9) . . ? C12 C7 P2 120.7(7) . . ? C8 C7 P2 121.2(7) . . ? C4 C5 C6 121.2(13) . . ? C15 C14 C13 121.2(11) . . ? C2 C3 C4 121.1(11) . . ? C12 C11 C10 120.1(11) . . ? C9 C10 C11 119.8(11) . . ? C20 C21 C22 120.3(10) . . ? C3 C2 C1 120.2(11) . . ? C5 C4 C3 118.8(11) . . ? C22 C23 C24 119.0(9) . . ? C23 C22 C21 120.5(10) . . ? C10 C9 C8 121.0(12) . . ? C16 C15 C14 120.2(12) . . ? C16 C17 C18 120.6(12) . . ? C9 C8 C7 120.5(10) . . ? C1 C6 C5 120.0(12) . . ? C17 C16 C15 121.0(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.758 _refine_diff_density_min -1.227 _refine_diff_density_rms 0.128 data_cuipph_cubic_203k _database_code_depnum_ccdc_archive 'CCDC 777562' #TrackingRef 'cubic-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method toluene/ether _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colorless _diffrn_ambient_temperature 203(1) _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 0.0021 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 0.2614 1.2674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7268 1.8135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0905 0.0944 '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' _symmetry_space_group_name_hall 'I -4bd 2c 3' _symmetry_int_tables_number 220 _chemical_absolute_configuration ad 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 29.9834(5) _cell_length_b 29.9834(5) _cell_length_c 29.9834(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26955.2(8) _cell_formula_units_Z 16 _cell_measurement_temperature 203(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14080 _exptl_absorpt_coefficient_mu 3.214 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6712 _exptl_absorpt_correction_T_max 0.6922 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal focus sealed tube' _diffrn_source_type 'Rigaku R-AXIS' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID-F' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22781 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6264 _reflns_number_gt 5155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_cell_refinement 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2006), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0507P)^2^+344.6059P] 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 0.02(4) _refine_ls_number_reflns 6264 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1458 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.003 _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 I2 I 0.991866(19) 0.037883(18) 0.921517(18) 0.03350(13) Uani 1 1 d . . . I1 I 1.054593(19) 0.054593(19) 1.054593(19) 0.0367(2) Uani 1 3 d S . . Cu1 Cu 0.96282(4) -0.03718(4) 0.96282(4) 0.0395(4) Uani 1 3 d S . . Cu2 Cu 1.05483(4) 0.01163(4) 0.97635(4) 0.0411(3) Uani 1 1 d . . . P1 P 0.91932(7) -0.08068(7) 0.91932(7) 0.0338(7) Uani 1 3 d S . . P2 P 1.12626(7) 0.00796(8) 0.95360(7) 0.0324(4) Uani 1 1 d . . . C12 C 1.1748(3) 0.0055(4) 1.0329(3) 0.046(2) Uani 1 1 d . . . H12 H 1.1694 0.0364 1.0343 0.055 Uiso 1 1 calc R . . C13 C 1.1567(3) 0.0597(3) 0.9419(3) 0.0356(18) Uani 1 1 d . . . C19 C 0.8594(3) -0.0699(3) 0.9240(3) 0.0325(17) Uani 1 1 d . . . C24 C 0.8268(3) -0.1019(3) 0.9167(3) 0.0385(19) Uani 1 1 d . . . H24 H 0.8353 -0.1306 0.9075 0.046 Uiso 1 1 calc R . . C1 C 1.1380(3) -0.0241(3) 0.9026(3) 0.0380(19) Uani 1 1 d . . . C20 C 0.8459(3) -0.0277(3) 0.9365(3) 0.043(2) Uani 1 1 d . . . H20 H 0.8674 -0.0054 0.9410 0.051 Uiso 1 1 calc R . . C18 C 1.1335(4) 0.0960(3) 0.9261(3) 0.046(2) Uani 1 1 d . . . H18 H 1.1022 0.0953 0.9245 0.055 Uiso 1 1 calc R . . C7 C 1.1598(3) -0.0192(3) 0.9964(3) 0.0348(18) Uani 1 1 d . . . C5 C 1.1885(5) -0.0547(6) 0.8487(5) 0.093(6) Uani 1 1 d . . . H5 H 1.2178 -0.0605 0.8394 0.112 Uiso 1 1 calc R . . C14 C 1.2031(3) 0.0621(4) 0.9456(4) 0.052(2) Uani 1 1 d . . . H14 H 1.2192 0.0382 0.9580 0.063 Uiso 1 1 calc R . . C3 C 1.1111(5) -0.0597(4) 0.8367(4) 0.063(3) Uani 1 1 d . . . H3 H 1.0869 -0.0688 0.8190 0.076 Uiso 1 1 calc R . . C11 C 1.1975(4) -0.0154(4) 1.0668(3) 0.053(3) Uani 1 1 d . . . H11 H 1.2081 0.0015 1.0909 0.064 Uiso 1 1 calc R . . C10 C 1.2048(4) -0.0604(5) 1.0660(4) 0.057(3) Uani 1 1 d . . . H10 H 1.2203 -0.0742 1.0895 0.068 Uiso 1 1 calc R . . C21 C 0.8005(4) -0.0175(4) 0.9425(4) 0.055(3) Uani 1 1 d . . . H21 H 0.7916 0.0113 0.9511 0.066 Uiso 1 1 calc R . . C2 C 1.1034(4) -0.0383(3) 0.8767(3) 0.046(2) Uani 1 1 d . . . H2 H 1.0740 -0.0333 0.8861 0.055 Uiso 1 1 calc R . . C4 C 1.1536(5) -0.0676(4) 0.8227(4) 0.068(4) Uani 1 1 d . . . H4 H 1.1588 -0.0819 0.7952 0.081 Uiso 1 1 calc R . . C23 C 0.7819(3) -0.0925(4) 0.9227(4) 0.049(2) Uani 1 1 d . . . H23 H 0.7602 -0.1146 0.9180 0.059 Uiso 1 1 calc R . . C22 C 0.7697(3) -0.0505(4) 0.9356(4) 0.051(2) Uani 1 1 d . . . H22 H 0.7393 -0.0440 0.9398 0.061 Uiso 1 1 calc R . . C9 C 1.1894(4) -0.0858(4) 1.0305(5) 0.065(3) Uani 1 1 d . . . H9 H 1.1942 -0.1168 1.0299 0.077 Uiso 1 1 calc R . . C15 C 1.2251(4) 0.0996(4) 0.9311(5) 0.067(4) Uani 1 1 d . . . H15 H 1.2564 0.1006 0.9325 0.081 Uiso 1 1 calc R . . C17 C 1.1569(5) 0.1339(4) 0.9123(4) 0.059(3) Uani 1 1 d . . . H17 H 1.1413 0.1587 0.9014 0.071 Uiso 1 1 calc R . . C8 C 1.1670(4) -0.0652(3) 0.9960(4) 0.049(2) Uani 1 1 d . . . H8 H 1.1564 -0.0824 0.9720 0.059 Uiso 1 1 calc R . . C6 C 1.1809(4) -0.0331(6) 0.8888(5) 0.084(5) Uani 1 1 d . . . H6 H 1.2052 -0.0245 0.9066 0.101 Uiso 1 1 calc R . . C16 C 1.2024(5) 0.1350(4) 0.9148(4) 0.060(3) Uani 1 1 d . . . H16 H 1.2180 0.1605 0.9051 0.072 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 I2 0.0347(3) 0.0335(3) 0.0323(3) 0.0019(2) -0.0021(2) -0.0004(2) I1 0.0367(2) 0.0367(2) 0.0367(2) -0.0037(2) -0.0037(2) -0.0037(2) Cu1 0.0395(4) 0.0395(4) 0.0395(4) -0.0031(4) -0.0031(4) -0.0031(4) Cu2 0.0300(5) 0.0542(7) 0.0392(6) 0.0005(5) 0.0013(4) 0.0019(5) P1 0.0338(7) 0.0338(7) 0.0338(7) -0.0011(9) -0.0011(9) -0.0011(9) P2 0.0271(9) 0.0374(11) 0.0327(11) -0.0015(9) 0.0009(8) 0.0002(8) C12 0.036(5) 0.056(6) 0.046(5) -0.009(4) -0.002(4) -0.004(4) C13 0.032(4) 0.034(4) 0.041(4) -0.007(4) 0.005(4) -0.004(3) C19 0.034(4) 0.035(4) 0.028(4) 0.001(3) -0.001(3) 0.002(3) C24 0.030(4) 0.037(4) 0.049(5) 0.002(4) -0.009(4) -0.007(3) C1 0.042(5) 0.041(5) 0.032(4) 0.000(3) -0.003(3) -0.008(4) C20 0.039(5) 0.037(5) 0.051(6) -0.006(4) -0.004(4) -0.001(4) C18 0.056(6) 0.037(5) 0.044(5) 0.000(4) 0.002(5) 0.007(4) C7 0.022(4) 0.042(5) 0.040(4) 0.002(4) 0.002(3) 0.007(3) C5 0.079(10) 0.120(13) 0.081(10) -0.059(10) 0.034(8) -0.029(9) C14 0.041(5) 0.051(6) 0.064(7) 0.007(5) 0.003(5) -0.010(4) C3 0.089(9) 0.057(7) 0.044(6) -0.020(5) -0.022(6) 0.012(6) C11 0.048(6) 0.081(8) 0.030(5) -0.009(5) -0.004(4) 0.010(5) C10 0.041(6) 0.085(9) 0.045(6) 0.016(6) -0.007(4) 0.010(5) C21 0.048(6) 0.050(6) 0.069(7) -0.008(5) 0.001(5) 0.012(5) C2 0.051(6) 0.040(5) 0.046(5) -0.008(4) -0.017(4) -0.001(4) C4 0.113(12) 0.055(7) 0.035(5) -0.016(5) 0.007(6) -0.014(7) C23 0.034(5) 0.054(6) 0.060(6) 0.001(5) -0.002(4) -0.009(4) C22 0.036(5) 0.062(6) 0.053(6) -0.001(5) -0.001(4) 0.009(5) C9 0.064(7) 0.053(7) 0.076(8) 0.005(6) -0.022(6) 0.014(6) C15 0.056(7) 0.061(8) 0.085(9) -0.004(7) 0.018(6) -0.014(6) C17 0.084(9) 0.040(6) 0.053(7) 0.002(5) 0.002(6) 0.002(6) C8 0.050(6) 0.042(5) 0.056(6) -0.004(4) -0.007(5) 0.011(4) C6 0.036(6) 0.143(14) 0.073(8) -0.063(9) 0.014(5) -0.021(7) C16 0.087(9) 0.040(5) 0.054(6) 0.001(5) 0.028(6) -0.026(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 I2 Cu2 2.6242(13) . ? I2 Cu1 2.7124(10) . ? I2 Cu2 2.7882(14) 17_546 ? I2 I2 4.3042(9) 9_645 ? I2 I1 4.4395(10) . ? I1 Cu2 2.6765(14) 17_546 ? I1 Cu2 2.6765(14) . ? I1 Cu2 2.6765(14) 9_645 ? Cu1 P1 2.259(4) . ? Cu1 I2 2.7124(10) 9_645 ? Cu1 I2 2.7124(10) 17_546 ? Cu1 Cu2 3.149(2) . ? Cu2 P2 2.251(2) . ? Cu2 I2 2.7882(14) 9_645 ? Cu2 Cu2 2.887(2) 17_546 ? Cu2 Cu2 2.887(2) 9_645 ? P1 C19 1.832(9) 9_645 ? P1 C19 1.832(9) . ? P1 C19 1.832(9) 17_546 ? P2 C7 1.822(9) . ? P2 C13 1.833(9) . ? P2 C1 1.840(9) . ? C12 C11 1.375(15) . ? C12 C7 1.396(13) . ? C13 C18 1.376(13) . ? C13 C14 1.398(14) . ? C19 C20 1.381(12) . ? C19 C24 1.386(12) . ? C24 C23 1.387(13) . ? C1 C2 1.364(12) . ? C1 C6 1.380(14) . ? C20 C21 1.404(14) . ? C18 C17 1.397(16) . ? C7 C8 1.397(13) . ? C5 C4 1.36(2) . ? C5 C6 1.382(16) . ? C14 C15 1.376(16) . ? C3 C4 1.36(2) . ? C3 C2 1.379(15) . ? C11 C10 1.367(17) . ? C10 C9 1.388(18) . ? C21 C22 1.368(16) . ? C23 C22 1.366(15) . ? C9 C8 1.378(15) . ? C15 C16 1.353(18) . ? C17 C16 1.367(18) . ? 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 Cu2 I2 Cu1 72.30(4) . . ? Cu2 I2 Cu2 64.38(5) . 17_546 ? Cu1 I2 Cu2 69.83(4) . 17_546 ? Cu2 I2 I2 38.67(3) . 9_645 ? Cu1 I2 I2 37.49(2) . 9_645 ? Cu2 I2 I2 74.12(2) 17_546 9_645 ? Cu2 I2 I1 33.49(3) . . ? Cu1 I2 I1 79.59(4) . . ? Cu2 I2 I1 34.84(3) 17_546 . ? I2 I2 I1 61.003(8) 9_645 . ? Cu2 I1 Cu2 65.27(4) 17_546 . ? Cu2 I1 Cu2 65.27(4) 17_546 9_645 ? Cu2 I1 Cu2 65.27(4) . 9_645 ? Cu2 I1 I2 36.52(3) 17_546 . ? Cu2 I1 I2 32.75(3) . . ? Cu2 I1 I2 72.51(3) 9_645 . ? P1 Cu1 I2 113.63(4) . 9_645 ? P1 Cu1 I2 113.63(4) . . ? I2 Cu1 I2 105.02(5) 9_645 . ? P1 Cu1 I2 113.63(4) . 17_546 ? I2 Cu1 I2 105.02(5) 9_645 17_546 ? I2 Cu1 I2 105.02(5) . 17_546 ? P1 Cu1 Cu2 148.04(3) . . ? I2 Cu1 Cu2 56.22(4) 9_645 . ? I2 Cu1 Cu2 52.55(4) . . ? I2 Cu1 Cu2 98.28(6) 17_546 . ? P2 Cu2 I2 120.63(8) . . ? P2 Cu2 I1 106.96(7) . . ? I2 Cu2 I1 113.76(5) . . ? P2 Cu2 I2 100.17(8) . 9_645 ? I2 Cu2 I2 105.32(5) . 9_645 ? I1 Cu2 I2 108.64(4) . 9_645 ? P2 Cu2 Cu2 155.33(8) . 17_546 ? I2 Cu2 Cu2 60.56(4) . 17_546 ? I1 Cu2 Cu2 57.36(2) . 17_546 ? I2 Cu2 Cu2 103.01(4) 9_645 17_546 ? P2 Cu2 Cu2 131.01(9) . 9_645 ? I2 Cu2 Cu2 107.33(4) . 9_645 ? I1 Cu2 Cu2 57.36(2) . 9_645 ? I2 Cu2 Cu2 55.05(4) 9_645 9_645 ? Cu2 Cu2 Cu2 60.0 17_546 9_645 ? P2 Cu2 Cu1 140.54(8) . . ? I2 Cu2 Cu1 55.15(3) . . ? I1 Cu2 Cu1 109.53(4) . . ? I2 Cu2 Cu1 53.95(2) 9_645 . ? Cu2 Cu2 Cu1 62.72(2) 17_546 . ? Cu2 Cu2 Cu1 62.72(2) 9_645 . ? C19 P1 C19 103.6(3) 9_645 . ? C19 P1 C19 103.6(3) 9_645 17_546 ? C19 P1 C19 103.6(3) . 17_546 ? C19 P1 Cu1 114.9(3) 9_645 . ? C19 P1 Cu1 114.9(3) . . ? C19 P1 Cu1 114.9(3) 17_546 . ? C7 P2 C13 103.8(4) . . ? C7 P2 C1 104.2(4) . . ? C13 P2 C1 100.8(4) . . ? C7 P2 Cu2 109.5(3) . . ? C13 P2 Cu2 119.4(3) . . ? C1 P2 Cu2 117.3(3) . . ? C11 C12 C7 119.7(10) . . ? C18 C13 C14 119.3(9) . . ? C18 C13 P2 119.0(7) . . ? C14 C13 P2 121.6(8) . . ? C20 C19 C24 118.1(8) . . ? C20 C19 P1 118.0(7) . . ? C24 C19 P1 123.9(7) . . ? C19 C24 C23 121.5(9) . . ? C2 C1 C6 118.4(10) . . ? C2 C1 P2 119.5(8) . . ? C6 C1 P2 122.1(7) . . ? C19 C20 C21 121.2(9) . . ? C13 C18 C17 119.4(11) . . ? C12 C7 C8 118.8(9) . . ? C12 C7 P2 119.5(7) . . ? C8 C7 P2 121.4(8) . . ? C4 C5 C6 120.4(14) . . ? C15 C14 C13 119.6(11) . . ? C4 C3 C2 120.4(11) . . ? C10 C11 C12 121.3(10) . . ? C11 C10 C9 119.9(10) . . ? C22 C21 C20 118.5(10) . . ? C1 C2 C3 121.0(11) . . ? C5 C4 C3 119.4(11) . . ? C22 C23 C24 118.9(9) . . ? C23 C22 C21 121.9(10) . . ? C8 C9 C10 119.5(11) . . ? C16 C15 C14 121.0(12) . . ? C16 C17 C18 120.4(11) . . ? C9 C8 C7 120.7(11) . . ? C1 C6 C5 120.4(12) . . ? C15 C16 C17 120.1(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.904 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.112 data_cuipph_cubic_153k _database_code_depnum_ccdc_archive 'CCDC 777563' #TrackingRef 'cubic-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method toluene/ether _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colorless _diffrn_ambient_temperature 153(1) _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 0.0021 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 0.2614 1.2674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7268 1.8135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0905 0.0944 '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' _symmetry_space_group_name_hall 'I -4bd 2c 3' _symmetry_int_tables_number 220 _chemical_absolute_configuration ad 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 29.9058(5) _cell_length_b 29.9058(5) _cell_length_c 29.9058(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26746.5(8) _cell_formula_units_Z 16 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14080 _exptl_absorpt_coefficient_mu 3.239 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6693 _exptl_absorpt_correction_T_max 0.6903 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal focus sealed tube' _diffrn_source_type 'Rigaku R-AXIS' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID-F' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47686 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6483 _reflns_number_gt 5667 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_cell_refinement 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2006), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0888P)^2^+400.4432P] 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 0.08(4) _refine_ls_number_reflns 6483 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1785 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.002 _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 I2 I 0.991680(19) 0.037969(18) 0.921228(18) 0.02694(13) Uani 1 1 d . . . I1 I 1.054878(19) 0.054878(19) 1.054878(19) 0.0292(2) Uani 1 3 d S . . Cu1 Cu 0.96292(4) -0.03708(4) 0.96292(4) 0.0311(4) Uani 1 3 d S . . Cu2 Cu 1.05454(4) 0.01161(4) 0.97650(4) 0.0318(3) Uani 1 1 d . . . P1 P 0.91935(7) -0.08065(7) 0.91935(7) 0.0270(7) Uani 1 3 d S . . P2 P 1.12603(7) 0.00777(8) 0.95370(7) 0.0259(4) Uani 1 1 d . . . C12 C 1.1743(3) 0.0052(4) 1.0333(3) 0.036(2) Uani 1 1 d . . . H12 H 1.1682 0.0364 1.0348 0.043 Uiso 1 1 calc R . . C13 C 1.1567(3) 0.0595(3) 0.9424(3) 0.0295(17) Uani 1 1 d . . . C19 C 0.8588(3) -0.0701(3) 0.9240(3) 0.0270(16) Uani 1 1 d . . . C24 C 0.8266(3) -0.1020(3) 0.9168(3) 0.0342(19) Uani 1 1 d . . . H24 H 0.8354 -0.1313 0.9081 0.041 Uiso 1 1 calc R . . C1 C 1.1382(3) -0.0245(3) 0.9028(3) 0.0325(19) Uani 1 1 d . . . C20 C 0.8456(3) -0.0280(3) 0.9370(4) 0.037(2) Uani 1 1 d . . . H20 H 0.8674 -0.0055 0.9422 0.044 Uiso 1 1 calc R . . C18 C 1.1333(4) 0.0961(4) 0.9261(3) 0.040(2) Uani 1 1 d . . . H18 H 1.1016 0.0956 0.9244 0.048 Uiso 1 1 calc R . . C7 C 1.1597(3) -0.0199(3) 0.9966(3) 0.0270(16) Uani 1 1 d . . . C5 C 1.1895(5) -0.0554(6) 0.8489(5) 0.074(5) Uani 1 1 d . . . H5 H 1.2193 -0.0616 0.8398 0.088 Uiso 1 1 calc R . . C14 C 1.2035(3) 0.0615(4) 0.9456(4) 0.041(2) Uani 1 1 d . . . H14 H 1.2197 0.0368 0.9574 0.049 Uiso 1 1 calc R . . C3 C 1.1107(5) -0.0604(4) 0.8363(4) 0.050(3) Uani 1 1 d . . . H3 H 1.0864 -0.0701 0.8184 0.060 Uiso 1 1 calc R . . C11 C 1.1977(4) -0.0157(4) 1.0672(3) 0.042(2) Uani 1 1 d . . . H11 H 1.2089 0.0015 1.0914 0.051 Uiso 1 1 calc R . . C10 C 1.2051(4) -0.0608(5) 1.0665(4) 0.048(3) Uani 1 1 d . . . H10 H 1.2209 -0.0748 1.0902 0.058 Uiso 1 1 calc R . . C21 C 0.8006(4) -0.0182(4) 0.9426(4) 0.044(2) Uani 1 1 d . . . H21 H 0.7917 0.0111 0.9511 0.053 Uiso 1 1 calc R . . C2 C 1.1028(4) -0.0387(3) 0.8762(3) 0.036(2) Uani 1 1 d . . . H2 H 1.0730 -0.0335 0.8856 0.043 Uiso 1 1 calc R . . C4 C 1.1537(5) -0.0680(4) 0.8225(4) 0.055(3) Uani 1 1 d . . . H4 H 1.1590 -0.0821 0.7945 0.066 Uiso 1 1 calc R . . C23 C 0.7814(3) -0.0927(4) 0.9219(4) 0.041(2) Uani 1 1 d . . . H23 H 0.7595 -0.1150 0.9159 0.049 Uiso 1 1 calc R . . C22 C 0.7689(4) -0.0505(4) 0.9358(4) 0.045(2) Uani 1 1 d . . . H22 H 0.7382 -0.0439 0.9408 0.054 Uiso 1 1 calc R . . C9 C 1.1895(4) -0.0859(4) 1.0308(5) 0.049(3) Uani 1 1 d . . . H9 H 1.1944 -0.1172 1.0300 0.059 Uiso 1 1 calc R . . C15 C 1.2260(4) 0.0991(4) 0.9317(5) 0.051(3) Uani 1 1 d . . . H15 H 1.2576 0.1000 0.9337 0.061 Uiso 1 1 calc R . . C17 C 1.1572(5) 0.1339(4) 0.9121(4) 0.045(2) Uani 1 1 d . . . H17 H 1.1414 0.1589 0.9006 0.054 Uiso 1 1 calc R . . C8 C 1.1668(4) -0.0653(3) 0.9965(4) 0.038(2) Uani 1 1 d . . . H8 H 1.1558 -0.0828 0.9723 0.046 Uiso 1 1 calc R . . C6 C 1.1811(4) -0.0335(6) 0.8892(5) 0.069(5) Uani 1 1 d . . . H6 H 1.2055 -0.0247 0.9076 0.083 Uiso 1 1 calc R . . C16 C 1.2030(5) 0.1356(4) 0.9147(4) 0.052(3) Uani 1 1 d . . . H16 H 1.2188 0.1614 0.9051 0.062 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 I2 0.0282(3) 0.0266(3) 0.0260(3) 0.0018(2) -0.00156(19) -0.0004(2) I1 0.0292(2) 0.0292(2) 0.0292(2) -0.0028(2) -0.0028(2) -0.0028(2) Cu1 0.0311(4) 0.0311(4) 0.0311(4) -0.0021(4) -0.0021(4) -0.0021(4) Cu2 0.0230(5) 0.0414(6) 0.0311(5) 0.0006(5) 0.0017(4) 0.0018(4) P1 0.0270(7) 0.0270(7) 0.0270(7) -0.0007(8) -0.0007(8) -0.0007(8) P2 0.0219(9) 0.0305(10) 0.0255(10) -0.0012(8) 0.0003(7) -0.0005(8) C12 0.033(4) 0.043(5) 0.031(4) -0.006(4) -0.005(4) 0.000(4) C13 0.028(4) 0.032(4) 0.029(4) -0.004(3) 0.001(3) 0.001(3) C19 0.028(4) 0.028(4) 0.025(4) 0.001(3) -0.002(3) 0.000(3) C24 0.031(4) 0.035(5) 0.036(5) 0.000(4) -0.001(4) -0.005(4) C1 0.028(4) 0.038(5) 0.031(4) -0.004(4) 0.002(3) -0.009(4) C20 0.035(5) 0.034(5) 0.041(5) -0.006(4) -0.003(4) 0.003(4) C18 0.044(5) 0.043(5) 0.033(5) 0.000(4) 0.007(4) 0.007(4) C7 0.020(4) 0.035(4) 0.026(4) -0.003(3) 0.000(3) -0.001(3) C5 0.057(8) 0.099(12) 0.066(9) -0.043(9) 0.029(7) -0.023(8) C14 0.032(5) 0.038(5) 0.053(6) 0.003(5) 0.004(4) -0.008(4) C3 0.066(8) 0.039(6) 0.044(6) -0.021(5) -0.015(5) 0.012(5) C11 0.038(5) 0.064(7) 0.026(4) 0.000(4) -0.006(4) 0.005(5) C10 0.033(5) 0.074(8) 0.037(5) 0.008(5) -0.007(4) 0.007(5) C21 0.040(5) 0.034(5) 0.058(7) -0.005(5) -0.009(5) 0.008(4) C2 0.043(5) 0.028(4) 0.038(5) -0.009(4) -0.013(4) 0.002(4) C4 0.085(10) 0.047(6) 0.032(5) -0.017(5) 0.010(6) -0.006(6) C23 0.026(4) 0.045(6) 0.052(6) 0.006(5) -0.006(4) -0.004(4) C22 0.033(5) 0.053(6) 0.048(6) 0.003(5) 0.000(4) 0.005(5) C9 0.046(6) 0.041(6) 0.060(7) 0.005(5) -0.011(5) 0.004(5) C15 0.041(6) 0.046(6) 0.064(8) -0.003(5) 0.011(5) -0.013(5) C17 0.063(7) 0.032(5) 0.040(6) -0.001(4) 0.000(5) -0.003(5) C8 0.034(5) 0.036(5) 0.045(6) 0.004(4) -0.006(4) 0.003(4) C6 0.033(6) 0.107(12) 0.067(8) -0.057(9) 0.009(5) -0.008(6) C16 0.085(9) 0.033(5) 0.037(5) 0.005(4) 0.021(6) -0.023(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 I2 Cu2 2.6246(13) . ? I2 Cu1 2.7077(10) . ? I2 Cu2 2.7852(14) 17_546 ? I2 I2 4.3063(10) 9_645 ? I2 I1 4.4501(10) . ? I1 Cu2 2.6774(14) . ? I1 Cu2 2.6774(14) 17_546 ? I1 Cu2 2.6774(14) 9_645 ? Cu1 P1 2.257(4) . ? Cu1 I2 2.7077(10) 9_645 ? Cu1 I2 2.7077(10) 17_546 ? Cu1 Cu2 3.129(2) . ? Cu2 P2 2.247(2) . ? Cu2 I2 2.7852(14) 9_645 ? Cu2 Cu2 2.863(2) 9_645 ? Cu2 Cu2 2.863(2) 17_546 ? P1 C19 1.843(9) 17_546 ? P1 C19 1.843(9) 9_645 ? P1 C19 1.843(9) . ? P2 C13 1.829(10) . ? P2 C7 1.831(9) . ? P2 C1 1.838(10) . ? C12 C11 1.382(14) . ? C12 C7 1.399(13) . ? C13 C18 1.390(14) . ? C13 C14 1.405(13) . ? C19 C24 1.374(13) . ? C19 C20 1.377(13) . ? C24 C23 1.389(14) . ? C1 C6 1.372(15) . ? C1 C2 1.391(13) . ? C20 C21 1.386(15) . ? C18 C17 1.399(16) . ? C7 C8 1.373(13) . ? C5 C4 1.38(2) . ? C5 C6 1.395(17) . ? C14 C15 1.373(15) . ? C3 C4 1.37(2) . ? C3 C2 1.379(15) . ? C11 C10 1.366(18) . ? C10 C9 1.386(18) . ? C21 C22 1.369(16) . ? C23 C22 1.381(17) . ? C9 C8 1.374(15) . ? C15 C16 1.386(19) . ? C17 C16 1.37(2) . ? 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 Cu2 I2 Cu1 71.85(4) . . ? Cu2 I2 Cu2 63.83(5) . 17_546 ? Cu1 I2 Cu2 69.44(4) . 17_546 ? Cu2 I2 I2 38.56(3) . 9_645 ? Cu1 I2 I2 37.33(2) . 9_645 ? Cu2 I2 I2 73.85(2) 17_546 9_645 ? Cu2 I2 I1 33.30(3) . . ? Cu1 I2 I1 79.37(4) . . ? Cu2 I2 I1 34.65(3) 17_546 . ? I2 I2 I1 61.063(8) 9_645 . ? Cu2 I1 Cu2 64.65(4) . 17_546 ? Cu2 I1 Cu2 64.65(4) . 9_645 ? Cu2 I1 Cu2 64.65(4) 17_546 9_645 ? Cu2 I1 I2 32.56(3) . . ? Cu2 I1 I2 36.26(3) 17_546 . ? Cu2 I1 I2 72.05(3) 9_645 . ? P1 Cu1 I2 113.34(4) . 9_645 ? P1 Cu1 I2 113.34(4) . . ? I2 Cu1 I2 105.35(5) 9_645 . ? P1 Cu1 I2 113.33(4) . 17_546 ? I2 Cu1 I2 105.35(5) 9_645 17_546 ? I2 Cu1 I2 105.35(5) . 17_546 ? P1 Cu1 Cu2 148.11(3) . . ? I2 Cu1 Cu2 56.44(4) 9_645 . ? I2 Cu1 Cu2 52.84(4) . . ? I2 Cu1 Cu2 98.50(6) 17_546 . ? P2 Cu2 I2 120.38(8) . . ? P2 Cu2 I1 106.66(7) . . ? I2 Cu2 I1 114.13(5) . . ? P2 Cu2 I2 99.74(8) . 9_645 ? I2 Cu2 I2 105.47(5) . 9_645 ? I1 Cu2 I2 109.09(4) . 9_645 ? P2 Cu2 Cu2 130.95(9) . 9_645 ? I2 Cu2 Cu2 107.60(4) . 9_645 ? I1 Cu2 Cu2 57.68(2) . 9_645 ? I2 Cu2 Cu2 55.36(4) 9_645 9_645 ? P2 Cu2 Cu2 155.47(8) . 17_546 ? I2 Cu2 Cu2 60.81(4) . 17_546 ? I1 Cu2 Cu2 57.68(2) . 17_546 ? I2 Cu2 Cu2 103.32(4) 9_645 17_546 ? Cu2 Cu2 Cu2 60.0 9_645 17_546 ? P2 Cu2 Cu1 140.35(8) . . ? I2 Cu2 Cu1 55.31(3) . . ? I1 Cu2 Cu1 109.99(4) . . ? I2 Cu2 Cu1 54.11(2) 9_645 . ? Cu2 Cu2 Cu1 62.78(2) 9_645 . ? Cu2 Cu2 Cu1 62.78(2) 17_546 . ? C19 P1 C19 103.2(3) 17_546 9_645 ? C19 P1 C19 103.2(3) 17_546 . ? C19 P1 C19 103.2(3) 9_645 . ? C19 P1 Cu1 115.1(3) 17_546 . ? C19 P1 Cu1 115.1(3) 9_645 . ? C19 P1 Cu1 115.1(3) . . ? C13 P2 C7 103.6(4) . . ? C13 P2 C1 101.1(4) . . ? C7 P2 C1 103.5(4) . . ? C13 P2 Cu2 119.3(3) . . ? C7 P2 Cu2 109.5(3) . . ? C1 P2 Cu2 117.8(3) . . ? C11 C12 C7 119.2(10) . . ? C18 C13 C14 119.5(10) . . ? C18 C13 P2 118.6(7) . . ? C14 C13 P2 121.5(8) . . ? C24 C19 C20 118.6(9) . . ? C24 C19 P1 124.0(7) . . ? C20 C19 P1 117.4(7) . . ? C19 C24 C23 121.8(10) . . ? C6 C1 C2 118.7(10) . . ? C6 C1 P2 122.3(8) . . ? C2 C1 P2 118.9(8) . . ? C19 C20 C21 120.4(10) . . ? C13 C18 C17 118.8(11) . . ? C8 C7 C12 119.1(9) . . ? C8 C7 P2 122.0(7) . . ? C12 C7 P2 118.5(7) . . ? C4 C5 C6 118.9(13) . . ? C15 C14 C13 120.1(11) . . ? C4 C3 C2 120.0(11) . . ? C10 C11 C12 121.2(10) . . ? C11 C10 C9 119.4(10) . . ? C22 C21 C20 120.4(10) . . ? C3 C2 C1 120.6(11) . . ? C3 C4 C5 120.6(11) . . ? C22 C23 C24 118.7(10) . . ? C21 C22 C23 120.1(10) . . ? C8 C9 C10 120.0(11) . . ? C14 C15 C16 120.9(12) . . ? C16 C17 C18 121.6(11) . . ? C7 C8 C9 121.0(11) . . ? C1 C6 C5 121.2(12) . . ? C17 C16 C15 119.0(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.002 _refine_diff_density_min -1.261 _refine_diff_density_rms 0.087 data_cuipph_cubic_105k _database_code_depnum_ccdc_archive 'CCDC 777564' #TrackingRef 'cubic-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method toluene/ether _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colorless _diffrn_ambient_temperature 105(1) _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 0.0021 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 0.2614 1.2674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7268 1.8135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0905 0.0944 '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' _symmetry_space_group_name_hall 'I -4bd 2c 3' _symmetry_int_tables_number 220 _chemical_absolute_configuration ad 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 29.8333(5) _cell_length_b 29.8333(5) _cell_length_c 29.8333(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26552.4(8) _cell_formula_units_Z 16 _cell_measurement_temperature 105(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14080 _exptl_absorpt_coefficient_mu 3.263 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6675 _exptl_absorpt_correction_T_max 0.6886 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal focus sealed tube' _diffrn_source_type 'Rigaku R-AXIS' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID-F' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60655 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6444 _reflns_number_gt 5950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_cell_refinement 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2006), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0990P)^2^+146.5832P] 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 0.08(3) _refine_ls_number_reflns 6444 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.003 _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 I2 I 0.991542(14) 0.038081(14) 0.920959(14) 0.01973(11) Uani 1 1 d . . . I1 I 1.055077(14) 0.055077(14) 1.055077(14) 0.02103(15) Uani 1 3 d S . . Cu1 Cu 0.96291(3) -0.03709(3) 0.96291(3) 0.0224(3) Uani 1 3 d S . . Cu2 Cu 1.05415(3) 0.01148(3) 0.97665(3) 0.02264(18) Uani 1 1 d . . . P1 P 0.91911(6) -0.08089(6) 0.91911(6) 0.0198(5) Uani 1 3 d S . . P2 P 1.12600(5) 0.00754(6) 0.95377(6) 0.0193(3) Uani 1 1 d . . . C12 C 1.1744(2) 0.0052(2) 1.0338(2) 0.0242(13) Uani 1 1 d . . . H12 H 1.1683 0.0364 1.0354 0.029 Uiso 1 1 calc R . . C13 C 1.1570(2) 0.0592(2) 0.9423(2) 0.0230(12) Uani 1 1 d . . . C19 C 0.8585(2) -0.0701(2) 0.9240(2) 0.0207(12) Uani 1 1 d . . . C24 C 0.8263(2) -0.1028(3) 0.9160(3) 0.0265(14) Uani 1 1 d . . . H24 H 0.8353 -0.1318 0.9065 0.032 Uiso 1 1 calc R . . C1 C 1.1380(2) -0.0249(2) 0.9028(2) 0.0229(13) Uani 1 1 d . . . C20 C 0.8452(3) -0.0274(3) 0.9369(2) 0.0266(14) Uani 1 1 d . . . H20 H 0.8671 -0.0047 0.9413 0.032 Uiso 1 1 calc R . . C18 C 1.1338(3) 0.0962(3) 0.9263(3) 0.0290(15) Uani 1 1 d . . . H18 H 1.1020 0.0959 0.9250 0.035 Uiso 1 1 calc R . . C7 C 1.1595(2) -0.0201(2) 0.9967(2) 0.0199(11) Uani 1 1 d . . . C5 C 1.1891(4) -0.0562(4) 0.8489(3) 0.053(3) Uani 1 1 d . . . H5 H 1.2189 -0.0634 0.8401 0.064 Uiso 1 1 calc R . . C14 C 1.2035(3) 0.0610(3) 0.9460(3) 0.0317(15) Uani 1 1 d . . . H14 H 1.2194 0.0363 0.9583 0.038 Uiso 1 1 calc R . . C3 C 1.1103(4) -0.0605(3) 0.8360(3) 0.042(2) Uani 1 1 d . . . H3 H 1.0858 -0.0699 0.8180 0.050 Uiso 1 1 calc R . . C11 C 1.1982(3) -0.0161(3) 1.0680(2) 0.0311(15) Uani 1 1 d . . . H11 H 1.2093 0.0011 1.0923 0.037 Uiso 1 1 calc R . . C10 C 1.2056(3) -0.0618(3) 1.0669(3) 0.0361(18) Uani 1 1 d . . . H10 H 1.2218 -0.0760 1.0903 0.043 Uiso 1 1 calc R . . C21 C 0.8002(3) -0.0178(3) 0.9433(3) 0.0334(16) Uani 1 1 d . . . H21 H 0.7913 0.0113 0.9526 0.040 Uiso 1 1 calc R . . C2 C 1.1028(3) -0.0389(3) 0.8761(3) 0.0282(14) Uani 1 1 d . . . H2 H 1.0729 -0.0335 0.8856 0.034 Uiso 1 1 calc R . . C4 C 1.1536(4) -0.0684(3) 0.8224(3) 0.043(2) Uani 1 1 d . . . H4 H 1.1590 -0.0825 0.7943 0.052 Uiso 1 1 calc R . . C23 C 0.7808(3) -0.0931(3) 0.9220(3) 0.0292(14) Uani 1 1 d . . . H23 H 0.7588 -0.1155 0.9164 0.035 Uiso 1 1 calc R . . C22 C 0.7681(3) -0.0506(3) 0.9361(3) 0.0315(15) Uani 1 1 d . . . H22 H 0.7373 -0.0440 0.9408 0.038 Uiso 1 1 calc R . . C9 C 1.1893(3) -0.0869(3) 1.0313(3) 0.0337(16) Uani 1 1 d . . . H9 H 1.1936 -0.1184 1.0307 0.040 Uiso 1 1 calc R . . C15 C 1.2267(3) 0.0985(3) 0.9320(3) 0.0382(18) Uani 1 1 d . . . H15 H 1.2585 0.0993 0.9342 0.046 Uiso 1 1 calc R . . C17 C 1.1575(3) 0.1337(3) 0.9120(3) 0.0313(15) Uani 1 1 d . . . H17 H 1.1416 0.1587 0.9002 0.038 Uiso 1 1 calc R . . C8 C 1.1666(3) -0.0660(2) 0.9965(3) 0.0279(14) Uani 1 1 d . . . H8 H 1.1557 -0.0835 0.9722 0.034 Uiso 1 1 calc R . . C6 C 1.1811(3) -0.0331(4) 0.8889(4) 0.052(3) Uani 1 1 d . . . H6 H 1.2056 -0.0230 0.9066 0.062 Uiso 1 1 calc R . . C16 C 1.2036(3) 0.1354(3) 0.9145(3) 0.0379(19) Uani 1 1 d . . . H16 H 1.2194 0.1612 0.9045 0.045 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 I2 0.0207(2) 0.01954(19) 0.01896(19) 0.00122(14) -0.00082(14) 0.00028(14) I1 0.02103(15) 0.02103(15) 0.02103(15) -0.00211(14) -0.00211(14) -0.00211(14) Cu1 0.0224(3) 0.0224(3) 0.0224(3) -0.0011(3) -0.0011(3) -0.0011(3) Cu2 0.0167(3) 0.0286(4) 0.0227(4) 0.0009(3) 0.0014(3) 0.0016(3) P1 0.0198(5) 0.0198(5) 0.0198(5) 0.0006(6) 0.0006(6) 0.0006(6) P2 0.0161(7) 0.0230(7) 0.0187(7) -0.0010(6) 0.0011(5) -0.0009(6) C12 0.024(3) 0.027(3) 0.021(3) -0.007(2) -0.005(2) -0.002(2) C13 0.018(3) 0.026(3) 0.025(3) -0.006(3) 0.002(2) 0.000(2) C19 0.021(3) 0.022(3) 0.019(3) -0.002(2) -0.004(2) -0.004(2) C24 0.023(3) 0.030(3) 0.027(3) 0.005(3) -0.002(3) -0.002(3) C1 0.024(3) 0.027(3) 0.018(3) -0.003(2) 0.003(2) -0.005(2) C20 0.028(3) 0.025(3) 0.027(3) -0.007(3) 0.000(3) -0.001(3) C18 0.031(4) 0.027(3) 0.028(3) 0.003(3) 0.003(3) 0.004(3) C7 0.019(3) 0.023(3) 0.018(3) -0.002(2) 0.004(2) 0.001(2) C5 0.046(5) 0.067(7) 0.047(5) -0.035(5) 0.025(4) -0.009(5) C14 0.026(3) 0.033(4) 0.036(4) 0.007(3) 0.002(3) -0.004(3) C3 0.057(6) 0.036(4) 0.033(4) -0.016(3) -0.016(4) 0.010(4) C11 0.028(3) 0.049(4) 0.016(3) -0.001(3) -0.005(2) -0.005(3) C10 0.025(3) 0.057(5) 0.027(4) 0.004(3) -0.003(3) 0.001(3) C21 0.026(3) 0.031(4) 0.042(4) -0.002(3) -0.003(3) 0.006(3) C2 0.029(3) 0.027(3) 0.029(4) -0.008(3) -0.003(3) 0.006(3) C4 0.070(6) 0.035(4) 0.026(4) -0.013(3) 0.011(4) -0.010(4) C23 0.025(3) 0.031(4) 0.032(4) 0.002(3) 0.001(3) -0.002(3) C22 0.025(3) 0.033(4) 0.036(4) -0.001(3) -0.004(3) 0.000(3) C9 0.029(4) 0.030(4) 0.042(4) 0.006(3) -0.011(3) 0.005(3) C15 0.033(4) 0.036(4) 0.045(5) 0.006(4) 0.007(3) -0.009(3) C17 0.040(4) 0.021(3) 0.033(4) 0.003(3) 0.001(3) 0.000(3) C8 0.027(3) 0.026(3) 0.031(4) 0.005(3) -0.001(3) -0.001(3) C6 0.028(4) 0.080(7) 0.048(5) -0.044(5) 0.012(4) -0.014(4) C16 0.056(5) 0.026(3) 0.032(4) 0.006(3) 0.016(4) -0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I2 Cu2 2.6228(10) . ? I2 Cu1 2.7066(7) . ? I2 Cu2 2.7786(10) 17_546 ? I2 I2 4.3094(7) 9_645 ? I2 I1 4.4564(7) . ? I1 Cu2 2.6771(11) 17_546 ? I1 Cu2 2.6771(11) . ? I1 Cu2 2.6771(11) 9_645 ? Cu1 P1 2.263(3) . ? Cu1 I2 2.7065(7) 17_546 ? Cu1 I2 2.7066(7) 9_645 ? Cu1 Cu2 3.1109(16) . ? Cu2 P2 2.2527(18) . ? Cu2 I2 2.7786(10) 9_645 ? Cu2 Cu2 2.8366(14) 17_546 ? Cu2 Cu2 2.8366(14) 9_645 ? P1 C19 1.843(7) 17_546 ? P1 C19 1.843(7) . ? P1 C19 1.843(7) 9_645 ? P2 C7 1.821(7) . ? P2 C13 1.829(7) . ? P2 C1 1.838(7) . ? C12 C11 1.395(10) . ? C12 C7 1.412(9) . ? C13 C18 1.386(10) . ? C13 C14 1.394(10) . ? C19 C20 1.386(10) . ? C19 C24 1.389(9) . ? C24 C23 1.399(10) . ? C1 C6 1.373(11) . ? C1 C2 1.381(10) . ? C20 C21 1.388(11) . ? C18 C17 1.391(11) . ? C7 C8 1.385(10) . ? C5 C4 1.370(15) . ? C5 C6 1.401(11) . ? C14 C15 1.380(11) . ? C3 C4 1.375(15) . ? C3 C2 1.379(11) . ? C11 C10 1.384(13) . ? C10 C9 1.387(12) . ? C21 C22 1.386(11) . ? C23 C22 1.389(11) . ? C9 C8 1.386(10) . ? C15 C16 1.400(13) . ? C17 C16 1.377(13) . ? 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 Cu2 I2 Cu1 71.41(3) . . ? Cu2 I2 Cu2 63.28(4) . 17_546 ? Cu1 I2 Cu2 69.09(3) . 17_546 ? Cu2 I2 I2 38.34(2) . 9_645 ? Cu1 I2 I2 37.241(17) . 9_645 ? Cu2 I2 I2 73.531(19) 17_546 9_645 ? Cu2 I2 I1 33.15(2) . . ? Cu1 I2 I1 79.24(3) . . ? Cu2 I2 I1 34.485(19) 17_546 . ? I2 I2 I1 61.085(6) 9_645 . ? Cu2 I1 Cu2 63.98(3) 17_546 . ? Cu2 I1 Cu2 63.98(3) 17_546 9_645 ? Cu2 I1 Cu2 63.98(3) . 9_645 ? Cu2 I1 I2 35.99(2) 17_546 . ? Cu2 I1 I2 32.39(2) . . ? Cu2 I1 I2 71.62(2) 9_645 . ? P1 Cu1 I2 113.18(3) . 17_546 ? P1 Cu1 I2 113.18(3) . . ? I2 Cu1 I2 105.52(3) 17_546 . ? P1 Cu1 I2 113.18(3) . 9_645 ? I2 Cu1 I2 105.52(3) 17_546 9_645 ? I2 Cu1 I2 105.52(3) . 9_645 ? P1 Cu1 Cu2 148.23(2) . . ? I2 Cu1 Cu2 98.53(5) 17_546 . ? I2 Cu1 Cu2 53.04(3) . . ? I2 Cu1 Cu2 56.55(3) 9_645 . ? P2 Cu2 I2 120.10(6) . . ? P2 Cu2 I1 106.28(5) . . ? I2 Cu2 I1 114.46(3) . . ? P2 Cu2 I2 99.31(6) . 9_645 ? I2 Cu2 I2 105.81(3) . 9_645 ? I1 Cu2 I2 109.53(3) . 9_645 ? P2 Cu2 Cu2 155.52(6) . 17_546 ? I2 Cu2 Cu2 61.04(3) . 17_546 ? I1 Cu2 Cu2 58.009(16) . 17_546 ? I2 Cu2 Cu2 103.71(3) 9_645 17_546 ? P2 Cu2 Cu2 130.91(6) . 9_645 ? I2 Cu2 Cu2 107.91(3) . 9_645 ? I1 Cu2 Cu2 58.009(16) . 9_645 ? I2 Cu2 Cu2 55.68(3) 9_645 9_645 ? Cu2 Cu2 Cu2 60.0 17_546 9_645 ? P2 Cu2 Cu1 140.21(6) . . ? I2 Cu2 Cu1 55.549(19) . . ? I1 Cu2 Cu1 110.52(3) . . ? I2 Cu2 Cu1 54.363(18) 9_645 . ? Cu2 Cu2 Cu1 62.876(18) 17_546 . ? Cu2 Cu2 Cu1 62.876(18) 9_645 . ? C19 P1 C19 103.6(3) 17_546 . ? C19 P1 C19 103.6(3) 17_546 9_645 ? C19 P1 C19 103.6(3) . 9_645 ? C19 P1 Cu1 114.8(2) 17_546 . ? C19 P1 Cu1 114.8(2) . . ? C19 P1 Cu1 114.8(2) 9_645 . ? C7 P2 C13 103.7(3) . . ? C7 P2 C1 103.7(3) . . ? C13 P2 C1 101.0(3) . . ? C7 P2 Cu2 109.4(2) . . ? C13 P2 Cu2 119.5(2) . . ? C1 P2 Cu2 117.6(2) . . ? C11 C12 C7 119.4(7) . . ? C18 C13 C14 119.5(7) . . ? C18 C13 P2 118.9(5) . . ? C14 C13 P2 121.4(6) . . ? C20 C19 C24 119.6(7) . . ? C20 C19 P1 117.6(5) . . ? C24 C19 P1 122.8(5) . . ? C19 C24 C23 120.3(7) . . ? C6 C1 C2 119.0(7) . . ? C6 C1 P2 121.7(6) . . ? C2 C1 P2 119.2(5) . . ? C19 C20 C21 120.4(7) . . ? C13 C18 C17 119.5(7) . . ? C8 C7 C12 118.9(7) . . ? C8 C7 P2 122.0(5) . . ? C12 C7 P2 118.8(5) . . ? C4 C5 C6 119.4(9) . . ? C15 C14 C13 120.5(8) . . ? C4 C3 C2 119.3(8) . . ? C10 C11 C12 120.8(7) . . ? C11 C10 C9 119.6(7) . . ? C22 C21 C20 120.0(7) . . ? C3 C2 C1 121.2(8) . . ? C5 C4 C3 120.7(8) . . ? C22 C23 C24 119.4(7) . . ? C21 C22 C23 120.3(7) . . ? C8 C9 C10 120.2(8) . . ? C14 C15 C16 120.1(8) . . ? C16 C17 C18 121.3(7) . . ? C7 C8 C9 121.0(7) . . ? C1 C6 C5 120.3(8) . . ? C17 C16 C15 118.9(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.542 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.084 data_cuipph_cubic_077k _database_code_depnum_ccdc_archive 'CCDC 777565' #TrackingRef 'cubic-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '?((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method toluene/ether _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colorless _diffrn_ambient_temperature 77(1) _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 0.0007 0.0011 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' H H 0.0000 0.0000 'International Tables Vol C Tables 6.1.1.4' Cu Cu 0.2733 0.9097 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' I I -1.0407 1.3054 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' P P 0.0618 0.0648 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I -4 3 d' _symmetry_space_group_name_hall 'I -4bd 2c 3' _symmetry_int_tables_number 220 _chemical_absolute_configuration ad 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 29.8024(5) _cell_length_b 29.8024(5) _cell_length_c 29.8024(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26470.0(8) _cell_formula_units_Z 16 _cell_measurement_temperature 77(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14080 _exptl_absorpt_coefficient_mu 1.89 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8234 _exptl_absorpt_correction_T_max 0.8977 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.5886 _diffrn_source 'SPring-8 BL02B1 bending magnet' _diffrn_source_type 'SPring-8 beamline BL02B1' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'SPring-8 BL02B1 Large cylindrical Image-Plate camera' _diffrn_measurement_method '\w axis scan' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 171294 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0119 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 24.47 _reflns_number_total 6455 _reflns_number_gt 6236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_cell_refinement 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2008), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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. Anomalous dispersion parameters are taken from S. Sasaki, KEK Report 88-14, 1-136 (1989). ; _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^)+(0.0185P)^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 0.014(9) _refine_ls_number_reflns 6455 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0124 _refine_ls_R_factor_gt 0.0119 _refine_ls_wR_factor_ref 0.0297 _refine_ls_wR_factor_gt 0.0297 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.015 _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 I2 I 0.991397(3) 0.038086(3) 0.920916(3) 0.01453(2) Uani 1 1 d . . . I1 I 1.055101(3) 0.055101(3) 1.055101(3) 0.01598(3) Uani 1 3 d S . . Cu1 Cu 0.962888(6) -0.037112(6) 0.962888(6) 0.01699(6) Uani 1 3 d S . . Cu2 Cu 1.053976(6) 0.011650(7) 0.976634(6) 0.01798(4) Uani 1 1 d . . . P1 P 0.918967(12) -0.081033(12) 0.918967(12) 0.01411(11) Uani 1 3 d S . . P2 P 1.125909(12) 0.007700(13) 0.953790(13) 0.01463(7) Uani 1 1 d . . . C12 C 1.17485(5) 0.00510(6) 1.03360(5) 0.0206(3) Uani 1 1 d . . . H12 H 1.1693 0.0365 1.0350 0.025 Uiso 1 1 calc R . . C13 C 1.15679(5) 0.05926(5) 0.94243(5) 0.0176(3) Uani 1 1 d . . . C19 C 0.85880(5) -0.07002(5) 0.92394(5) 0.0159(3) Uani 1 1 d . . . C24 C 0.82607(5) -0.10278(5) 0.91591(5) 0.0184(3) Uani 1 1 d . . . H24 H 0.8348 -0.1319 0.9062 0.022 Uiso 1 1 calc R . . C1 C 1.13752(5) -0.02452(5) 0.90286(5) 0.0182(3) Uani 1 1 d . . . C20 C 0.84529(5) -0.02736(5) 0.93704(5) 0.0212(3) Uani 1 1 d . . . H20 H 0.8671 -0.0046 0.9417 0.025 Uiso 1 1 calc R . . C18 C 1.13367(6) 0.09635(6) 0.92596(5) 0.0216(3) Uani 1 1 d . . . H18 H 1.1018 0.0959 0.9245 0.026 Uiso 1 1 calc R . . C7 C 1.15946(5) -0.01971(5) 0.99680(5) 0.0158(3) Uani 1 1 d . . . C5 C 1.18928(8) -0.05550(9) 0.84859(7) 0.0473(6) Uani 1 1 d . . . H5 H 1.2192 -0.0614 0.8394 0.057 Uiso 1 1 calc R . . C14 C 1.20366(6) 0.06129(6) 0.94555(6) 0.0246(3) Uani 1 1 d . . . H14 H 1.2198 0.0365 0.9574 0.030 Uiso 1 1 calc R . . C3 C 1.11018(7) -0.06068(6) 0.83579(6) 0.0317(4) Uani 1 1 d . . . H3 H 1.0856 -0.0701 0.8177 0.038 Uiso 1 1 calc R . . C11 C 1.19813(6) -0.01589(6) 1.06807(5) 0.0251(3) Uani 1 1 d . . . H11 H 1.2089 0.0012 1.0927 0.030 Uiso 1 1 calc R . . C10 C 1.20565(6) -0.06190(6) 1.06659(6) 0.0267(4) Uani 1 1 d . . . H10 H 1.2218 -0.0762 1.0900 0.032 Uiso 1 1 calc R . . C21 C 0.79988(6) -0.01755(6) 0.94340(6) 0.0260(3) Uani 1 1 d . . . H21 H 0.7910 0.0117 0.9525 0.031 Uiso 1 1 calc R . . C2 C 1.10236(6) -0.03866(5) 0.87618(6) 0.0230(3) Uani 1 1 d . . . H2 H 1.0724 -0.0333 0.8856 0.028 Uiso 1 1 calc R . . C4 C 1.15376(7) -0.06887(6) 0.82188(6) 0.0352(4) Uani 1 1 d . . . H4 H 1.1592 -0.0836 0.7941 0.042 Uiso 1 1 calc R . . C23 C 0.78078(5) -0.09284(6) 0.92214(6) 0.0220(3) Uani 1 1 d . . . H23 H 0.7587 -0.1151 0.9166 0.026 Uiso 1 1 calc R . . C22 C 0.76791(5) -0.05058(6) 0.93643(6) 0.0241(3) Uani 1 1 d . . . H22 H 0.7371 -0.0442 0.9415 0.029 Uiso 1 1 calc R . . C9 C 1.18954(6) -0.08663(6) 1.03100(6) 0.0292(4) Uani 1 1 d . . . H9 H 1.1943 -0.1181 1.0301 0.035 Uiso 1 1 calc R . . C15 C 1.22659(6) 0.09911(6) 0.93154(6) 0.0296(4) Uani 1 1 d . . . H15 H 1.2584 0.1001 0.9339 0.035 Uiso 1 1 calc R . . C17 C 1.15732(7) 0.13423(6) 0.91159(6) 0.0273(4) Uani 1 1 d . . . H17 H 1.1414 0.1593 0.8999 0.033 Uiso 1 1 calc R . . C8 C 1.16632(6) -0.06580(5) 0.99634(6) 0.0234(3) Uani 1 1 d . . . H8 H 1.1550 -0.0832 0.9721 0.028 Uiso 1 1 calc R . . C6 C 1.18122(7) -0.03350(8) 0.88873(7) 0.0427(6) Uani 1 1 d . . . H6 H 1.2058 -0.0244 0.9069 0.051 Uiso 1 1 calc R . . C16 C 1.20364(7) 0.13549(6) 0.91421(6) 0.0311(4) Uani 1 1 d . . . H16 H 1.2196 0.1612 0.9042 0.037 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 I2 0.01499(4) 0.01474(4) 0.01386(4) 0.00078(3) -0.00140(3) -0.00028(3) I1 0.01598(3) 0.01598(3) 0.01598(3) -0.00205(3) -0.00205(3) -0.00205(3) Cu1 0.01699(6) 0.01699(6) 0.01699(6) -0.00181(6) -0.00181(6) -0.00181(6) Cu2 0.01348(8) 0.02344(10) 0.01703(9) 0.00047(7) 0.00050(7) 0.00146(7) P1 0.01411(11) 0.01411(11) 0.01411(11) -0.00136(13) -0.00136(13) -0.00136(13) P2 0.01313(16) 0.01666(17) 0.01409(17) -0.00124(13) 0.00009(13) -0.00002(13) C12 0.0196(7) 0.0241(8) 0.0180(7) -0.0034(6) -0.0001(6) 0.0016(6) C13 0.0196(7) 0.0180(7) 0.0153(7) -0.0014(6) 0.0022(5) -0.0009(5) C19 0.0162(7) 0.0176(7) 0.0139(6) 0.0000(5) -0.0015(5) 0.0003(5) C24 0.0183(7) 0.0177(7) 0.0192(7) -0.0005(6) -0.0012(6) -0.0012(6) C1 0.0204(7) 0.0203(7) 0.0140(7) -0.0025(5) 0.0015(5) -0.0034(6) C20 0.0196(7) 0.0199(7) 0.0242(8) -0.0036(6) -0.0044(6) -0.0001(6) C18 0.0239(8) 0.0225(8) 0.0182(7) -0.0023(6) 0.0016(6) 0.0014(6) C7 0.0115(6) 0.0213(7) 0.0145(6) -0.0004(5) 0.0008(5) 0.0012(5) C5 0.0383(11) 0.0612(15) 0.0426(12) -0.0296(11) 0.0225(10) -0.0174(10) C14 0.0202(8) 0.0236(8) 0.0301(9) 0.0014(7) 0.0036(7) -0.0040(6) C3 0.0459(11) 0.0230(9) 0.0263(9) -0.0084(7) -0.0154(8) 0.0055(7) C11 0.0212(8) 0.0391(10) 0.0151(7) -0.0039(6) 0.0003(6) 0.0035(7) C10 0.0221(8) 0.0369(10) 0.0211(8) 0.0069(7) -0.0003(6) 0.0060(7) C21 0.0242(8) 0.0225(8) 0.0314(9) -0.0048(7) -0.0034(7) 0.0043(6) C2 0.0270(8) 0.0177(7) 0.0244(8) -0.0030(6) -0.0072(6) 0.0035(6) C4 0.0567(13) 0.0283(9) 0.0207(9) -0.0079(7) 0.0080(8) -0.0077(9) C23 0.0171(7) 0.0243(8) 0.0248(8) 0.0040(6) -0.0004(6) -0.0019(6) C22 0.0176(7) 0.0300(8) 0.0248(8) 0.0018(7) -0.0003(6) 0.0042(6) C9 0.0291(9) 0.0234(8) 0.0352(10) 0.0035(7) -0.0054(7) 0.0059(7) C15 0.0225(8) 0.0295(9) 0.0367(10) 0.0004(7) 0.0081(7) -0.0070(7) C17 0.0423(11) 0.0183(8) 0.0215(8) -0.0008(6) 0.0027(7) 0.0015(7) C8 0.0211(8) 0.0231(8) 0.0259(8) -0.0026(6) -0.0025(6) 0.0019(6) C6 0.0237(9) 0.0665(15) 0.0381(11) -0.0314(10) 0.0087(8) -0.0121(9) C16 0.0430(11) 0.0235(8) 0.0267(9) -0.0021(7) 0.0125(8) -0.0106(8) _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 I2 Cu2 2.6185(2) . ? I2 Cu1 2.70350(17) . ? I2 Cu2 2.7803(2) 17_546 ? I2 I2 4.30603(17) 9_645 ? I2 I1 4.45576(17) . ? I1 Cu2 2.6733(2) . ? I1 Cu2 2.6733(2) 17_546 ? I1 Cu2 2.6733(2) 9_645 ? Cu1 P1 2.2672(7) . ? Cu1 I2 2.70350(17) 17_546 ? Cu1 I2 2.70350(17) 9_645 ? Cu1 Cu2 3.1063(4) . ? Cu2 P2 2.2523(4) . ? Cu2 I2 2.7803(2) 9_645 ? Cu2 Cu2 2.8272(3) 17_546 ? Cu2 Cu2 2.8272(3) 9_645 ? P1 C19 1.8289(15) . ? P1 C19 1.8289(15) 17_546 ? P1 C19 1.8289(15) 9_645 ? P2 C7 1.8192(15) . ? P2 C13 1.8230(16) . ? P2 C1 1.8292(16) . ? C12 C11 1.389(2) . ? C12 C7 1.400(2) . ? C13 C18 1.392(2) . ? C13 C14 1.401(2) . ? C19 C20 1.390(2) . ? C19 C24 1.401(2) . ? C24 C23 1.394(2) . ? C1 C2 1.381(2) . ? C1 C6 1.395(2) . ? C20 C21 1.397(2) . ? C18 C17 1.398(2) . ? C7 C8 1.389(2) . ? C5 C4 1.383(3) . ? C5 C6 1.385(3) . ? C14 C15 1.383(2) . ? C3 C4 1.385(3) . ? C3 C2 1.390(2) . ? C11 C10 1.390(3) . ? C10 C9 1.378(3) . ? C21 C22 1.386(2) . ? C23 C22 1.384(2) . ? C9 C8 1.390(2) . ? C15 C16 1.382(3) . ? C17 C16 1.383(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu2 I2 Cu1 71.398(7) . . ? Cu2 I2 Cu2 63.076(8) . 17_546 ? Cu1 I2 Cu2 68.989(7) . 17_546 ? Cu2 I2 I2 38.418(5) . 9_645 ? Cu1 I2 I2 37.214(4) . 9_645 ? Cu2 I2 I2 73.431(4) 17_546 9_645 ? Cu2 I2 I1 33.029(4) . . ? Cu1 I2 I1 79.221(7) . . ? Cu2 I2 I1 34.426(4) 17_546 . ? I2 I2 I1 61.105(1) 9_645 . ? Cu2 I1 Cu2 63.847(7) . 17_546 ? Cu2 I1 Cu2 63.847(7) . 9_645 ? Cu2 I1 Cu2 63.847(7) 17_546 9_645 ? Cu2 I1 I2 32.268(5) . . ? Cu2 I1 I2 36.012(5) 17_546 . ? Cu2 I1 I2 71.507(5) 9_645 . ? P1 Cu1 I2 113.135(7) . 17_546 ? P1 Cu1 I2 113.135(7) . . ? I2 Cu1 I2 105.572(8) 17_546 . ? P1 Cu1 I2 113.135(7) . 9_645 ? I2 Cu1 I2 105.572(8) 17_546 9_645 ? I2 Cu1 I2 105.572(8) . 9_645 ? P1 Cu1 Cu2 148.299(5) . . ? I2 Cu1 Cu2 98.512(10) 17_546 . ? I2 Cu1 Cu2 53.027(6) . . ? I2 Cu1 Cu2 56.673(6) 9_645 . ? P2 Cu2 I2 120.130(12) . . ? P2 Cu2 I1 106.129(12) . . ? I2 Cu2 I1 114.703(8) . . ? P2 Cu2 I2 99.156(12) . 9_645 ? I2 Cu2 I2 105.764(8) . 9_645 ? I1 Cu2 I2 109.562(7) . 9_645 ? P2 Cu2 Cu2 155.626(13) . 17_546 ? I2 Cu2 Cu2 61.258(7) . 17_546 ? I1 Cu2 Cu2 58.076(4) . 17_546 ? I2 Cu2 Cu2 103.689(6) 9_645 17_546 ? P2 Cu2 Cu2 130.677(14) . 9_645 ? I2 Cu2 Cu2 108.077(6) . 9_645 ? I1 Cu2 Cu2 58.076(4) . 9_645 ? I2 Cu2 Cu2 55.666(7) 9_645 9_645 ? Cu2 Cu2 Cu2 60.0 17_546 9_645 ? P2 Cu2 Cu1 140.128(13) . . ? I2 Cu2 Cu1 55.575(4) . . ? I1 Cu2 Cu1 110.666(7) . . ? I2 Cu2 Cu1 54.338(4) 9_645 . ? Cu2 Cu2 Cu1 62.929(4) 17_546 . ? Cu2 Cu2 Cu1 62.930(4) 9_645 . ? C19 P1 C19 103.93(6) . 17_546 ? C19 P1 C19 103.93(6) . 9_645 ? C19 P1 C19 103.93(6) 17_546 9_645 ? C19 P1 Cu1 114.57(5) . . ? C19 P1 Cu1 114.57(5) 17_546 . ? C19 P1 Cu1 114.57(5) 9_645 . ? C7 P2 C13 103.41(7) . . ? C7 P2 C1 104.18(7) . . ? C13 P2 C1 101.12(7) . . ? C7 P2 Cu2 109.49(5) . . ? C13 P2 Cu2 119.51(5) . . ? C1 P2 Cu2 117.28(5) . . ? C11 C12 C7 120.35(15) . . ? C18 C13 C14 118.86(15) . . ? C18 C13 P2 119.01(12) . . ? C14 C13 P2 121.82(12) . . ? C20 C19 C24 118.93(14) . . ? C20 C19 P1 118.10(12) . . ? C24 C19 P1 122.96(11) . . ? C23 C24 C19 120.22(14) . . ? C2 C1 C6 118.44(15) . . ? C2 C1 P2 119.62(13) . . ? C6 C1 P2 121.87(13) . . ? C19 C20 C21 120.68(15) . . ? C13 C18 C17 119.99(16) . . ? C8 C7 C12 118.80(14) . . ? C8 C7 P2 121.20(12) . . ? C12 C7 P2 119.66(12) . . ? C4 C5 C6 120.1(2) . . ? C15 C14 C13 120.52(17) . . ? C4 C3 C2 119.97(17) . . ? C12 C11 C10 120.10(16) . . ? C9 C10 C11 119.72(16) . . ? C22 C21 C20 119.80(15) . . ? C1 C2 C3 120.99(17) . . ? C5 C4 C3 119.65(17) . . ? C22 C23 C24 120.19(15) . . ? C23 C22 C21 120.13(15) . . ? C10 C9 C8 120.46(16) . . ? C16 C15 C14 120.51(17) . . ? C16 C17 C18 120.51(17) . . ? C7 C8 C9 120.51(16) . . ? C5 C6 C1 120.89(18) . . ? C15 C16 C17 119.58(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.256 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.039 data_cuipph_cubic_045k _database_code_depnum_ccdc_archive 'CCDC 777566' #TrackingRef 'cubic-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method toluene/ether _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colorless _diffrn_ambient_temperature 45(1) _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 0.0007 0.0011 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' H H 0.0000 0.0000 'International Tables Vol C Tables 6.1.1.4' Cu Cu 0.2733 0.9097 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' I I -1.0407 1.3054 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' P P 0.0618 0.0648 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I -4 3 d' _symmetry_space_group_name_hall 'I -4bd 2c 3' _symmetry_int_tables_number 220 _chemical_absolute_configuration ad 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 29.7569(5) _cell_length_b 29.7569(5) _cell_length_c 29.7569(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26348.9(8) _cell_formula_units_Z 16 _cell_measurement_temperature 45(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14080 _exptl_absorpt_coefficient_mu 1.89 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8227 _exptl_absorpt_correction_T_max 0.8973 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.5886 _diffrn_source 'SPring-8 BL02B1 bending magnet' _diffrn_source_type 'SPring-8 beamline BL02B1' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'SPring-8 BL02B1 Large cylindrical Image-Plate camera' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 170976 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0116 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 24.47 _reflns_number_total 6439 _reflns_number_gt 6277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_cell_refinement 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2008), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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. Anomalous dispersion parameters are taken from S. Sasaki, KEK Report 88-14, 1-136 (1989). ; _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^)+(0.0180P)^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 0.017(8) _refine_ls_number_reflns 6439 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0118 _refine_ls_R_factor_gt 0.0114 _refine_ls_wR_factor_ref 0.0288 _refine_ls_wR_factor_gt 0.0288 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.006 _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 I2 I 0.991215(3) 0.038128(3) 0.920656(3) 0.00982(2) Uani 1 1 d . . . I1 I 1.055187(3) 0.055187(3) 1.055187(3) 0.01082(3) Uani 1 3 d S . . Cu1 Cu 0.962887(6) -0.037113(6) 0.962887(6) 0.01168(6) Uani 1 3 d S . . Cu2 Cu 1.053692(6) 0.011550(6) 0.976659(6) 0.01224(4) Uani 1 1 d . . . P1 P 0.918877(12) -0.081123(12) 0.918877(12) 0.00988(11) Uani 1 3 d S . . P2 P 1.125784(12) 0.007531(12) 0.953902(12) 0.01027(7) Uani 1 1 d . . . C12 C 1.17479(5) 0.00491(5) 1.03389(5) 0.0148(3) Uani 1 1 d . . . H12 H 1.1693 0.0363 1.0353 0.018 Uiso 1 1 calc R . . C13 C 1.15691(5) 0.05911(5) 0.94256(5) 0.0125(3) Uani 1 1 d . . . C19 C 0.85864(5) -0.07011(5) 0.92386(5) 0.0115(3) Uani 1 1 d . . . C24 C 0.82582(5) -0.10292(5) 0.91582(5) 0.0134(3) Uani 1 1 d . . . H24 H 0.8345 -0.1320 0.9060 0.016 Uiso 1 1 calc R . . C1 C 1.13756(5) -0.02481(5) 0.90290(5) 0.0130(3) Uani 1 1 d . . . C20 C 0.84507(5) -0.02727(5) 0.93714(5) 0.0149(3) Uani 1 1 d . . . H20 H 0.8670 -0.0045 0.9418 0.018 Uiso 1 1 calc R . . C18 C 1.13381(5) 0.09636(5) 0.92590(5) 0.0157(3) Uani 1 1 d . . . H18 H 1.1019 0.0960 0.9244 0.019 Uiso 1 1 calc R . . C7 C 1.15930(5) -0.01999(5) 0.99704(5) 0.0113(3) Uani 1 1 d . . . C5 C 1.18957(7) -0.05601(7) 0.84872(6) 0.0329(5) Uani 1 1 d . . . H5 H 1.2196 -0.0621 0.8396 0.039 Uiso 1 1 calc R . . C14 C 1.20386(5) 0.06089(5) 0.94574(5) 0.0172(3) Uani 1 1 d . . . H14 H 1.2199 0.0360 0.9577 0.021 Uiso 1 1 calc R . . C3 C 1.11015(6) -0.06086(5) 0.83556(6) 0.0224(3) Uani 1 1 d . . . H3 H 1.0856 -0.0702 0.8174 0.027 Uiso 1 1 calc R . . C11 C 1.19815(5) -0.01610(6) 1.06845(5) 0.0173(3) Uani 1 1 d . . . H11 H 1.2090 0.0011 1.0931 0.021 Uiso 1 1 calc R . . C10 C 1.20568(5) -0.06223(6) 1.06698(5) 0.0186(3) Uani 1 1 d . . . H10 H 1.2220 -0.0765 1.0904 0.022 Uiso 1 1 calc R . . C21 C 0.79962(5) -0.01748(5) 0.94369(5) 0.0183(3) Uani 1 1 d . . . H21 H 0.7907 0.0118 0.9529 0.022 Uiso 1 1 calc R . . C2 C 1.10218(5) -0.03879(5) 0.87601(5) 0.0166(3) Uani 1 1 d . . . H2 H 1.0721 -0.0332 0.8853 0.020 Uiso 1 1 calc R . . C4 C 1.15384(6) -0.06923(6) 0.82174(6) 0.0251(4) Uani 1 1 d . . . H4 H 1.1593 -0.0839 0.7939 0.030 Uiso 1 1 calc R . . C23 C 0.78042(5) -0.09306(5) 0.92221(5) 0.0155(3) Uani 1 1 d . . . H23 H 0.7583 -0.1154 0.9166 0.019 Uiso 1 1 calc R . . C22 C 0.76752(5) -0.05076(5) 0.93670(5) 0.0171(3) Uani 1 1 d . . . H22 H 0.7367 -0.0444 0.9419 0.021 Uiso 1 1 calc R . . C9 C 1.18931(6) -0.08722(5) 1.03127(6) 0.0203(3) Uani 1 1 d . . . H9 H 1.1940 -0.1188 1.0305 0.024 Uiso 1 1 calc R . . C15 C 1.22708(6) 0.09872(6) 0.93162(6) 0.0205(3) Uani 1 1 d . . . H15 H 1.2589 0.0996 0.9340 0.025 Uiso 1 1 calc R . . C17 C 1.15766(6) 0.13417(5) 0.91143(5) 0.0188(3) Uani 1 1 d . . . H17 H 1.1419 0.1593 0.8997 0.023 Uiso 1 1 calc R . . C8 C 1.16610(5) -0.06625(5) 0.99660(5) 0.0166(3) Uani 1 1 d . . . H8 H 1.1548 -0.0837 0.9724 0.020 Uiso 1 1 calc R . . C6 C 1.18142(6) -0.03395(7) 0.88899(6) 0.0297(4) Uani 1 1 d . . . H6 H 1.2060 -0.0250 0.9073 0.036 Uiso 1 1 calc R . . C16 C 1.20415(6) 0.13522(5) 0.91408(5) 0.0214(3) Uani 1 1 d . . . H16 H 1.2202 0.1609 0.9039 0.026 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 I2 0.01013(4) 0.00994(4) 0.00940(4) 0.00050(3) -0.00085(3) -0.00018(3) I1 0.01082(3) 0.01082(3) 0.01082(3) -0.00137(3) -0.00137(3) -0.00137(3) Cu1 0.01168(6) 0.01168(6) 0.01168(6) -0.00109(6) -0.00109(6) -0.00109(6) Cu2 0.00932(8) 0.01580(8) 0.01159(8) 0.00041(6) 0.00040(6) 0.00095(6) P1 0.00988(11) 0.00988(11) 0.00988(11) -0.00079(12) -0.00079(12) -0.00079(12) P2 0.00935(15) 0.01158(16) 0.00989(16) -0.00077(12) 0.00013(12) 0.00001(12) C12 0.0140(6) 0.0170(7) 0.0133(6) -0.0025(5) -0.0001(5) 0.0010(5) C13 0.0143(6) 0.0128(6) 0.0106(6) -0.0008(5) 0.0017(5) -0.0006(5) C19 0.0116(6) 0.0130(6) 0.0098(6) 0.0004(5) -0.0009(5) 0.0003(5) C24 0.0139(7) 0.0127(6) 0.0134(6) -0.0007(5) -0.0008(5) -0.0007(5) C1 0.0151(7) 0.0144(6) 0.0097(6) -0.0016(5) 0.0010(5) -0.0023(5) C20 0.0141(7) 0.0141(7) 0.0166(7) -0.0026(5) -0.0027(5) -0.0005(5) C18 0.0169(7) 0.0171(7) 0.0131(7) -0.0017(5) 0.0009(5) 0.0011(5) C7 0.0083(6) 0.0157(6) 0.0100(6) 0.0000(5) 0.0006(4) 0.0008(5) C5 0.0272(9) 0.0412(11) 0.0303(10) -0.0187(8) 0.0163(8) -0.0122(8) C14 0.0143(7) 0.0166(7) 0.0208(7) 0.0008(6) 0.0022(6) -0.0022(5) C3 0.0324(9) 0.0159(7) 0.0190(8) -0.0055(6) -0.0113(7) 0.0037(6) C11 0.0148(7) 0.0265(8) 0.0105(6) -0.0024(5) 0.0007(5) 0.0024(6) C10 0.0150(7) 0.0259(8) 0.0149(7) 0.0051(6) 0.0001(5) 0.0040(6) C21 0.0179(7) 0.0162(7) 0.0209(7) -0.0035(6) -0.0021(6) 0.0026(6) C2 0.0195(7) 0.0126(6) 0.0178(7) -0.0020(5) -0.0051(6) 0.0035(5) C4 0.0409(10) 0.0200(8) 0.0145(7) -0.0052(6) 0.0056(7) -0.0054(7) C23 0.0129(7) 0.0170(7) 0.0166(7) 0.0028(5) 0.0000(5) -0.0009(5) C22 0.0131(7) 0.0216(7) 0.0168(7) 0.0014(6) -0.0001(5) 0.0027(6) C9 0.0199(8) 0.0162(7) 0.0247(8) 0.0023(6) -0.0028(6) 0.0037(6) C15 0.0157(7) 0.0209(8) 0.0248(8) 0.0005(6) 0.0052(6) -0.0045(6) C17 0.0281(8) 0.0133(7) 0.0150(7) -0.0006(5) 0.0019(6) 0.0012(6) C8 0.0145(7) 0.0166(7) 0.0186(7) -0.0019(5) -0.0011(5) 0.0009(5) C6 0.0174(8) 0.0440(11) 0.0277(9) -0.0212(8) 0.0062(7) -0.0082(7) C16 0.0293(9) 0.0167(7) 0.0183(7) -0.0011(6) 0.0081(6) -0.0066(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 I2 Cu2 2.6190(2) . ? I2 Cu1 2.70232(16) . ? I2 Cu2 2.7781(2) 17_546 ? I2 I2 4.31002(17) 9_645 ? I2 I1 4.46175(17) . ? I1 Cu2 2.6737(2) . ? I1 Cu2 2.6737(2) 9_645 ? I1 Cu2 2.6737(2) 17_546 ? Cu1 P1 2.2683(7) . ? Cu1 I2 2.70232(16) 17_546 ? Cu1 I2 2.70232(16) 9_645 ? Cu1 Cu2 3.0929(3) . ? Cu2 P2 2.2527(4) . ? Cu2 I2 2.7781(2) 9_645 ? Cu2 Cu2 2.8116(3) 9_645 ? Cu2 Cu2 2.8116(3) 17_546 ? P1 C19 1.8282(14) . ? P1 C19 1.8282(14) 9_645 ? P1 C19 1.8282(14) 17_546 ? P2 C7 1.8202(14) . ? P2 C13 1.8242(15) . ? P2 C1 1.8309(15) . ? C12 C11 1.390(2) . ? C12 C7 1.401(2) . ? C13 C18 1.395(2) . ? C13 C14 1.401(2) . ? C19 C20 1.394(2) . ? C19 C24 1.4015(19) . ? C24 C23 1.396(2) . ? C1 C2 1.386(2) . ? C1 C6 1.396(2) . ? C20 C21 1.397(2) . ? C18 C17 1.398(2) . ? C7 C8 1.391(2) . ? C5 C6 1.388(2) . ? C5 C4 1.389(3) . ? C14 C15 1.386(2) . ? C3 C4 1.386(3) . ? C3 C2 1.392(2) . ? C11 C10 1.392(2) . ? C10 C9 1.386(2) . ? C21 C22 1.392(2) . ? C23 C22 1.385(2) . ? C9 C8 1.389(2) . ? C15 C16 1.385(2) . ? C17 C16 1.386(2) . ? 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 Cu2 I2 Cu1 71.055(7) . . ? Cu2 I2 Cu2 62.711(8) . 17_546 ? Cu1 I2 Cu2 68.699(7) . 17_546 ? Cu2 I2 I2 38.297(5) . 9_645 ? Cu1 I2 I2 37.111(4) . 9_645 ? Cu2 I2 I2 73.228(4) 17_546 9_645 ? Cu2 I2 I1 32.920(4) . . ? Cu1 I2 I1 79.054(6) . . ? Cu2 I2 I1 34.311(4) 17_546 . ? I2 I2 I1 61.119(1) 9_645 . ? Cu2 I1 Cu2 63.443(7) . 9_645 ? Cu2 I1 Cu2 63.443(7) . 17_546 ? Cu2 I1 Cu2 63.443(7) 9_645 17_546 ? Cu2 I1 I2 32.164(4) . . ? Cu2 I1 I2 71.242(5) 9_645 . ? Cu2 I1 I2 35.852(4) 17_546 . ? P1 Cu1 I2 112.952(6) . . ? P1 Cu1 I2 112.952(7) . 17_546 ? I2 Cu1 I2 105.778(7) . 17_546 ? P1 Cu1 I2 112.952(6) . 9_645 ? I2 Cu1 I2 105.778(7) . 9_645 ? I2 Cu1 I2 105.778(7) 17_546 9_645 ? P1 Cu1 Cu2 148.342(5) . . ? I2 Cu1 Cu2 53.216(6) . . ? I2 Cu1 Cu2 98.653(10) 17_546 . ? I2 Cu1 Cu2 56.809(6) 9_645 . ? P2 Cu2 I2 120.050(12) . . ? P2 Cu2 I1 105.823(11) . . ? I2 Cu2 I1 114.915(7) . . ? P2 Cu2 I2 98.856(12) . 9_645 ? I2 Cu2 I2 105.954(7) . 9_645 ? I1 Cu2 I2 109.837(6) . 9_645 ? P2 Cu2 Cu2 130.557(13) . 9_645 ? I2 Cu2 Cu2 108.281(6) . 9_645 ? I1 Cu2 Cu2 58.278(3) . 9_645 ? I2 Cu2 Cu2 55.874(6) 9_645 9_645 ? P2 Cu2 Cu2 155.653(12) . 17_546 ? I2 Cu2 Cu2 61.415(7) . 17_546 ? I1 Cu2 Cu2 58.278(4) . 17_546 ? I2 Cu2 Cu2 103.930(6) 9_645 17_546 ? Cu2 Cu2 Cu2 60.0 9_645 17_546 ? P2 Cu2 Cu1 140.108(12) . . ? I2 Cu2 Cu1 55.730(4) . . ? I1 Cu2 Cu1 110.960(7) . . ? I2 Cu2 Cu1 54.492(4) 9_645 . ? Cu2 Cu2 Cu1 62.965(4) 9_645 . ? Cu2 Cu2 Cu1 62.965(4) 17_546 . ? C19 P1 C19 103.93(5) . 9_645 ? C19 P1 C19 103.93(5) . 17_546 ? C19 P1 C19 103.93(5) 9_645 17_546 ? C19 P1 Cu1 114.57(5) . . ? C19 P1 Cu1 114.57(5) 9_645 . ? C19 P1 Cu1 114.57(5) 17_546 . ? C7 P2 C13 103.34(7) . . ? C7 P2 C1 104.07(7) . . ? C13 P2 C1 101.06(7) . . ? C7 P2 Cu2 109.50(5) . . ? C13 P2 Cu2 119.63(5) . . ? C1 P2 Cu2 117.34(5) . . ? C11 C12 C7 120.37(14) . . ? C18 C13 C14 119.02(14) . . ? C18 C13 P2 118.95(11) . . ? C14 C13 P2 121.70(11) . . ? C20 C19 C24 118.91(13) . . ? C20 C19 P1 118.08(11) . . ? C24 C19 P1 122.99(11) . . ? C23 C24 C19 120.32(13) . . ? C2 C1 C6 118.71(14) . . ? C2 C1 P2 119.40(12) . . ? C6 C1 P2 121.82(12) . . ? C19 C20 C21 120.70(14) . . ? C13 C18 C17 119.92(15) . . ? C8 C7 C12 118.86(13) . . ? C8 C7 P2 121.22(11) . . ? C12 C7 P2 119.60(11) . . ? C6 C5 C4 119.95(18) . . ? C15 C14 C13 120.48(15) . . ? C4 C3 C2 120.09(15) . . ? C12 C11 C10 120.07(14) . . ? C9 C10 C11 119.79(14) . . ? C22 C21 C20 119.69(14) . . ? C1 C2 C3 120.76(15) . . ? C3 C4 C5 119.70(16) . . ? C22 C23 C24 120.13(14) . . ? C23 C22 C21 120.21(14) . . ? C10 C9 C8 120.22(15) . . ? C16 C15 C14 120.38(15) . . ? C16 C17 C18 120.49(15) . . ? C9 C8 C7 120.64(14) . . ? C5 C6 C1 120.78(16) . . ? C15 C16 C17 119.69(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.215 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.041 data_cuipph_cubic_020k _database_code_depnum_ccdc_archive 'CCDC 777567' #TrackingRef 'cubic-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method toluene/ether _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colorless _diffrn_ambient_temperature 11(1) _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 0.0007 0.0011 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' H H 0.0000 0.0000 'International Tables Vol C Tables 6.1.1.4' Cu Cu 0.2733 0.9097 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' I I -1.0407 1.3054 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' P P 0.0618 0.0648 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I -4 3 d' _symmetry_space_group_name_hall 'I -4bd 2c 3' _symmetry_int_tables_number 220 _chemical_absolute_configuration ad 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 29.7325(5) _cell_length_b 29.7325(5) _cell_length_c 29.7325(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26284.2(8) _cell_formula_units_Z 16 _cell_measurement_temperature 20(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14080 _exptl_absorpt_coefficient_mu 1.90 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8223 _exptl_absorpt_correction_T_max 0.8970 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.5886 _diffrn_source 'SPring-8 BL02B1 bending magnet' _diffrn_source_type 'SPring-8 beamline BL02B1' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'SPring-8 BL02B1 Large cylindrical Image-Plate camera' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 170782 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 24.48 _reflns_number_total 6421 _reflns_number_gt 6262 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_cell_refinement 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2008), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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. Anomalous dispersion parameters are taken from S. Sasaki, KEK Report 88-14, 1-136 (1989). ; _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^)+(0.0216P)^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 0.015(9) _refine_ls_number_reflns 6421 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0135 _refine_ls_R_factor_gt 0.0131 _refine_ls_wR_factor_ref 0.0327 _refine_ls_wR_factor_gt 0.0326 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.011 _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 I2 I 0.991044(3) 0.038122(3) 0.920448(3) 0.00670(2) Uani 1 1 d . . . I1 I 1.055181(3) 0.055181(3) 1.055181(3) 0.00733(3) Uani 1 3 d S . . Cu1 Cu 0.962849(7) -0.037151(7) 0.962849(7) 0.00830(6) Uani 1 3 d S . . Cu2 Cu 1.053488(6) 0.011438(7) 0.976597(6) 0.00856(4) Uani 1 1 d . . . P1 P 0.918797(13) -0.081203(13) 0.918797(13) 0.00705(11) Uani 1 3 d S . . P2 P 1.125697(13) 0.007347(13) 0.953993(13) 0.00732(7) Uani 1 1 d . . . C12 C 1.17467(5) 0.00475(5) 1.03411(5) 0.0107(3) Uani 1 1 d . . . H12 H 1.1691 0.0362 1.0355 0.013 Uiso 1 1 calc R . . C13 C 1.15701(5) 0.05890(5) 0.94262(5) 0.0094(3) Uani 1 1 d . . . C19 C 0.85851(5) -0.07020(5) 0.92378(5) 0.0086(3) Uani 1 1 d . . . C24 C 0.82568(5) -0.10306(5) 0.91576(5) 0.0099(3) Uani 1 1 d . . . H24 H 0.8344 -0.1321 0.9058 0.012 Uiso 1 1 calc R . . C1 C 1.13764(5) -0.02511(5) 0.90300(5) 0.0094(3) Uani 1 1 d . . . C20 C 0.84495(5) -0.02729(5) 0.93712(5) 0.0108(3) Uani 1 1 d . . . H20 H 0.8669 -0.0045 0.9417 0.013 Uiso 1 1 calc R . . C18 C 1.13395(6) 0.09622(6) 0.92583(5) 0.0118(3) Uani 1 1 d . . . H18 H 1.1020 0.0959 0.9243 0.014 Uiso 1 1 calc R . . C7 C 1.15915(5) -0.02025(5) 0.99725(5) 0.0083(3) Uani 1 1 d . . . C5 C 1.18993(7) -0.05656(7) 0.84898(6) 0.0223(4) Uani 1 1 d . . . H5 H 1.2200 -0.0628 0.8400 0.027 Uiso 1 1 calc R . . C14 C 1.20402(5) 0.06049(5) 0.94593(6) 0.0124(3) Uani 1 1 d . . . H14 H 1.2199 0.0355 0.9580 0.015 Uiso 1 1 calc R . . C3 C 1.11029(6) -0.06087(6) 0.83530(6) 0.0162(3) Uani 1 1 d . . . H3 H 1.0858 -0.0700 0.8169 0.019 Uiso 1 1 calc R . . C11 C 1.19812(5) -0.01627(6) 1.06864(5) 0.0126(3) Uani 1 1 d . . . H11 H 1.2091 0.0009 1.0932 0.015 Uiso 1 1 calc R . . C10 C 1.20556(5) -0.06257(6) 1.06727(6) 0.0134(3) Uani 1 1 d . . . H10 H 1.2219 -0.0769 1.0907 0.016 Uiso 1 1 calc R . . C21 C 0.79945(6) -0.01749(6) 0.94378(6) 0.0137(3) Uani 1 1 d . . . H21 H 0.7905 0.0118 0.9529 0.016 Uiso 1 1 calc R . . C2 C 1.10215(6) -0.03877(5) 0.87578(6) 0.0125(3) Uani 1 1 d . . . H2 H 1.0721 -0.0330 0.8849 0.015 Uiso 1 1 calc R . . C4 C 1.15410(7) -0.06956(6) 0.82171(6) 0.0182(3) Uani 1 1 d . . . H4 H 1.1596 -0.0843 0.7939 0.022 Uiso 1 1 calc R . . C23 C 0.78019(5) -0.09327(5) 0.92230(6) 0.0118(3) Uani 1 1 d . . . H23 H 0.7581 -0.1157 0.9167 0.014 Uiso 1 1 calc R . . C22 C 0.76730(5) -0.05087(6) 0.93692(5) 0.0125(3) Uani 1 1 d . . . H22 H 0.7364 -0.0446 0.9423 0.015 Uiso 1 1 calc R . . C9 C 1.18904(6) -0.08760(6) 1.03151(6) 0.0144(3) Uani 1 1 d . . . H9 H 1.1936 -0.1192 1.0308 0.017 Uiso 1 1 calc R . . C15 C 1.22746(6) 0.09832(6) 0.93172(6) 0.0147(3) Uani 1 1 d . . . H15 H 1.2593 0.0991 0.9341 0.018 Uiso 1 1 calc R . . C17 C 1.15788(6) 0.13401(6) 0.91132(6) 0.0136(3) Uani 1 1 d . . . H17 H 1.1422 0.1592 0.8995 0.016 Uiso 1 1 calc R . . C8 C 1.16586(6) -0.06661(5) 0.99672(6) 0.0122(3) Uani 1 1 d . . . H8 H 1.1545 -0.0840 0.9724 0.015 Uiso 1 1 calc R . . C6 C 1.18161(6) -0.03448(7) 0.88937(6) 0.0204(4) Uani 1 1 d . . . H6 H 1.2061 -0.0257 0.9079 0.025 Uiso 1 1 calc R . . C16 C 1.20461(6) 0.13489(6) 0.91404(6) 0.0155(3) Uani 1 1 d . . . H16 H 1.2208 0.1605 0.9038 0.019 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 I2 0.00687(4) 0.00678(4) 0.00645(4) 0.00033(3) -0.00050(3) -0.00007(3) I1 0.00733(3) 0.00733(3) 0.00733(3) -0.00089(3) -0.00089(3) -0.00089(3) Cu1 0.00830(6) 0.00830(6) 0.00830(6) -0.00072(6) -0.00072(6) -0.00072(6) Cu2 0.00669(8) 0.01084(9) 0.00814(8) 0.00026(7) 0.00025(7) 0.00072(7) P1 0.00705(11) 0.00705(11) 0.00705(11) -0.00047(13) -0.00047(13) -0.00047(13) P2 0.00680(16) 0.00807(17) 0.00708(17) -0.00047(13) 0.00004(13) 0.00007(13) C12 0.0104(7) 0.0121(7) 0.0095(7) -0.0015(5) 0.0000(5) 0.0007(5) C13 0.0105(7) 0.0098(7) 0.0080(6) -0.0007(5) 0.0013(5) -0.0006(5) C19 0.0090(7) 0.0096(7) 0.0071(6) 0.0007(5) 0.0001(5) 0.0007(5) C24 0.0109(7) 0.0096(7) 0.0093(7) -0.0005(5) -0.0005(5) -0.0005(6) C1 0.0107(7) 0.0107(7) 0.0070(6) -0.0011(5) 0.0009(5) -0.0012(5) C20 0.0109(7) 0.0101(7) 0.0115(7) -0.0010(5) -0.0008(5) -0.0001(5) C18 0.0120(7) 0.0130(7) 0.0102(7) -0.0003(6) 0.0008(6) 0.0008(6) C7 0.0063(6) 0.0116(7) 0.0070(6) 0.0005(5) -0.0001(5) 0.0004(5) C5 0.0188(9) 0.0272(10) 0.0209(9) -0.0107(8) 0.0098(7) -0.0062(7) C14 0.0106(7) 0.0123(7) 0.0143(7) 0.0006(6) 0.0012(6) -0.0013(5) C3 0.0215(9) 0.0127(8) 0.0143(8) -0.0035(6) -0.0077(6) 0.0022(6) C11 0.0112(7) 0.0185(8) 0.0080(7) -0.0014(6) 0.0008(5) 0.0009(6) C10 0.0105(7) 0.0190(8) 0.0106(7) 0.0037(6) 0.0004(5) 0.0025(6) C21 0.0134(7) 0.0130(7) 0.0148(7) -0.0021(6) -0.0013(6) 0.0023(6) C2 0.0145(8) 0.0095(7) 0.0134(8) -0.0013(6) -0.0029(6) 0.0024(6) C4 0.0288(10) 0.0148(8) 0.0109(8) -0.0033(6) 0.0037(7) -0.0033(7) C23 0.0102(7) 0.0131(7) 0.0123(7) 0.0026(5) 0.0004(6) -0.0005(5) C22 0.0095(7) 0.0158(7) 0.0121(7) 0.0012(6) 0.0008(5) 0.0016(6) C9 0.0147(8) 0.0107(7) 0.0176(8) 0.0014(6) -0.0010(6) 0.0024(6) C15 0.0112(7) 0.0158(8) 0.0170(8) -0.0002(6) 0.0036(6) -0.0026(6) C17 0.0195(8) 0.0100(7) 0.0113(7) -0.0006(6) 0.0009(6) 0.0010(6) C8 0.0112(7) 0.0124(7) 0.0129(7) -0.0013(6) -0.0010(6) 0.0003(6) C6 0.0119(8) 0.0294(10) 0.0200(9) -0.0131(7) 0.0032(6) -0.0047(7) C16 0.0203(8) 0.0129(7) 0.0135(8) -0.0004(6) 0.0056(6) -0.0043(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 I2 Cu2 2.6198(2) . ? I2 Cu1 2.70205(17) . ? I2 Cu2 2.7771(2) 17_546 ? I2 I2 4.31352(18) 9_645 ? I2 I1 4.46556(18) . ? I1 Cu2 2.6746(2) 17_546 ? I1 Cu2 2.6745(2) . ? I1 Cu2 2.6745(2) 9_645 ? Cu1 P1 2.2686(7) . ? Cu1 I2 2.70204(18) 17_546 ? Cu1 I2 2.70205(18) 9_645 ? Cu1 Cu2 3.0849(4) . ? Cu2 P2 2.2530(4) . ? Cu2 I2 2.7771(2) 9_645 ? Cu2 Cu2 2.8041(3) 9_645 ? Cu2 Cu2 2.8041(3) 17_546 ? P1 C19 1.8281(15) 17_546 ? P1 C19 1.8281(15) 9_645 ? P1 C19 1.8281(15) . ? P2 C7 1.8213(16) . ? P2 C13 1.8250(16) . ? P2 C1 1.8319(16) . ? C12 C11 1.390(2) . ? C12 C7 1.402(2) . ? C13 C18 1.397(2) . ? C13 C14 1.402(2) . ? C19 C20 1.396(2) . ? C19 C24 1.401(2) . ? C24 C23 1.397(2) . ? C1 C2 1.391(2) . ? C1 C6 1.397(2) . ? C20 C21 1.398(2) . ? C18 C17 1.398(2) . ? C7 C8 1.393(2) . ? C5 C6 1.391(2) . ? C5 C4 1.394(3) . ? C14 C15 1.389(2) . ? C3 C4 1.388(3) . ? C3 C2 1.392(2) . ? C11 C10 1.395(2) . ? C10 C9 1.388(2) . ? C21 C22 1.393(2) . ? C23 C22 1.388(2) . ? C9 C8 1.391(2) . ? C15 C16 1.386(2) . ? C17 C16 1.392(2) . ? 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 Cu2 I2 Cu1 70.835(7) . . ? Cu2 I2 Cu2 62.526(8) . 17_546 ? Cu1 I2 Cu2 68.515(7) . 17_546 ? Cu2 I2 I2 38.216(5) . 9_645 ? Cu1 I2 I2 37.042(4) . 9_645 ? Cu2 I2 I2 73.117(4) 17_546 9_645 ? Cu2 I2 I1 32.873(4) . . ? Cu1 I2 I1 78.931(7) . . ? Cu2 I2 I1 34.255(4) 17_546 . ? I2 I2 I1 61.120(1) 9_645 . ? Cu2 I1 Cu2 63.231(7) 17_546 . ? Cu2 I1 Cu2 63.231(8) 17_546 9_645 ? Cu2 I1 Cu2 63.231(8) . 9_645 ? Cu2 I1 I2 35.765(5) 17_546 . ? Cu2 I1 I2 32.118(5) . . ? Cu2 I1 I2 71.110(5) 9_645 . ? P1 Cu1 I2 112.828(7) . 17_546 ? P1 Cu1 I2 112.828(7) . . ? I2 Cu1 I2 105.916(8) 17_546 . ? P1 Cu1 I2 112.828(7) . 9_645 ? I2 Cu1 I2 105.916(8) 17_546 9_645 ? I2 Cu1 I2 105.916(8) . 9_645 ? P1 Cu1 Cu2 148.346(5) . . ? I2 Cu1 Cu2 98.774(11) 17_546 . ? I2 Cu1 Cu2 53.338(6) . . ? I2 Cu1 Cu2 56.895(6) 9_645 . ? P2 Cu2 I2 120.105(13) . . ? P2 Cu2 I1 105.600(12) . . ? I2 Cu2 I1 115.009(8) . . ? P2 Cu2 I2 98.645(13) . 9_645 ? I2 Cu2 I2 106.081(8) . 9_645 ? I1 Cu2 I2 109.979(7) . 9_645 ? P2 Cu2 Cu2 130.402(14) . 9_645 ? I2 Cu2 Cu2 108.388(6) . 9_645 ? I1 Cu2 Cu2 58.385(4) . 9_645 ? I2 Cu2 Cu2 55.989(7) 9_645 9_645 ? P2 Cu2 Cu2 155.674(13) . 17_546 ? I2 Cu2 Cu2 61.485(7) . 17_546 ? I1 Cu2 Cu2 58.385(4) . 17_546 ? I2 Cu2 Cu2 104.068(6) 9_645 17_546 ? Cu2 Cu2 Cu2 60.000(1) 9_645 17_546 ? P2 Cu2 Cu1 140.144(13) . . ? I2 Cu2 Cu1 55.827(4) . . ? I1 Cu2 Cu1 111.095(7) . . ? I2 Cu2 Cu1 54.590(4) 9_645 . ? Cu2 Cu2 Cu1 62.969(4) 9_645 . ? Cu2 Cu2 Cu1 62.969(4) 17_546 . ? C19 P1 C19 103.91(6) 17_546 9_645 ? C19 P1 C19 103.91(6) 17_546 . ? C19 P1 C19 103.91(6) 9_645 . ? C19 P1 Cu1 114.59(5) 17_546 . ? C19 P1 Cu1 114.59(5) 9_645 . ? C19 P1 Cu1 114.59(5) . . ? C7 P2 C13 103.33(7) . . ? C7 P2 C1 103.96(7) . . ? C13 P2 C1 100.97(7) . . ? C7 P2 Cu2 109.52(5) . . ? C13 P2 Cu2 119.74(5) . . ? C1 P2 Cu2 117.39(5) . . ? C11 C12 C7 120.27(15) . . ? C18 C13 C14 119.20(15) . . ? C18 C13 P2 118.88(12) . . ? C14 C13 P2 121.60(12) . . ? C20 C19 C24 118.98(14) . . ? C20 C19 P1 118.02(12) . . ? C24 C19 P1 122.98(12) . . ? C23 C24 C19 120.35(14) . . ? C2 C1 C6 118.88(15) . . ? C2 C1 P2 119.24(12) . . ? C6 C1 P2 121.78(12) . . ? C19 C20 C21 120.69(15) . . ? C13 C18 C17 119.92(15) . . ? C8 C7 C12 119.10(14) . . ? C8 C7 P2 121.06(12) . . ? C12 C7 P2 119.53(12) . . ? C6 C5 C4 119.83(18) . . ? C15 C14 C13 120.42(16) . . ? C4 C3 C2 120.18(16) . . ? C12 C11 C10 120.12(15) . . ? C9 C10 C11 119.72(15) . . ? C22 C21 C20 119.66(15) . . ? C1 C2 C3 120.60(16) . . ? C3 C4 C5 119.75(16) . . ? C22 C23 C24 120.02(15) . . ? C23 C22 C21 120.25(15) . . ? C10 C9 C8 120.30(15) . . ? C16 C15 C14 120.31(16) . . ? C16 C17 C18 120.34(16) . . ? C9 C8 C7 120.43(15) . . ? C5 C6 C1 120.75(17) . . ? C15 C16 C17 119.78(16) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.259 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.063 # Attachment 'mono-combined.cif.txt' data_cuipph_mono_294k _database_code_depnum_ccdc_archive 'CCDC 777568' #TrackingRef 'mono-combined.cif.txt' _audit_update_record ; 2009-12-07 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method chloroform/ether _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 294(1) _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 0.0021 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 0.2614 1.2674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7268 1.8135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0905 0.0944 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 13.5413(10) _cell_length_b 26.949(2) _cell_length_c 19.4847(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.0220(10) _cell_angle_gamma 90.00 _cell_volume 7022.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 294(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 3.084 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7018 _exptl_absorpt_correction_T_max 0.8191 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co. Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal focus sealed tube' _diffrn_source_type 'Rigaku SCX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCX' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65738 _diffrn_reflns_av_R_equivalents 0.0918 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15986 _reflns_number_gt 8863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystal Clear (Rigaku & MSC Co. Ltd., 2006)' _computing_cell_refinement 'Crystal Clear (Rigaku & MSC Co. Ltd., 2006)' _computing_data_reduction 'Crysatal Clear (Rigaku & MSC Co. Ltd., 2006), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0232P)^2^+6.9036P] 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 15986 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I4 I 0.48024(3) -0.198999(14) 0.34551(2) 0.04588(11) Uani 1 1 d . . . I3 I 0.17211(3) -0.191334(15) 0.22161(2) 0.05220(12) Uani 1 1 d . . . I2 I 0.42939(3) -0.138423(14) 0.13377(2) 0.04739(11) Uani 1 1 d . . . I1 I 0.32254(3) -0.063025(14) 0.31484(2) 0.04900(11) Uani 1 1 d . . . Cu1 Cu 0.36589(5) -0.20630(3) 0.22168(4) 0.0543(2) Uani 1 1 d . . . Cu4 Cu 0.29508(6) -0.16101(3) 0.33795(4) 0.0581(2) Uani 1 1 d . . . Cu2 Cu 0.47094(5) -0.11464(3) 0.26927(4) 0.0521(2) Uani 1 1 d . . . Cu3 Cu 0.27416(5) -0.10981(3) 0.19344(4) 0.0559(2) Uani 1 1 d . . . P1 P 0.39612(11) -0.28165(5) 0.17936(8) 0.0427(4) Uani 1 1 d . . . P4 P 0.24392(12) -0.17595(6) 0.44102(9) 0.0508(4) Uani 1 1 d . . . P2 P 0.61437(11) -0.07049(6) 0.28745(8) 0.0429(4) Uani 1 1 d . . . P3 P 0.17213(11) -0.06500(6) 0.11442(8) 0.0475(4) Uani 1 1 d . . . C10 C 0.2474(5) -0.4159(3) 0.2667(5) 0.088(3) Uani 1 1 d . . . H10 H 0.2192 -0.4432 0.2855 0.105 Uiso 1 1 calc R . . C58 C 0.0778(7) -0.3239(3) 0.4574(5) 0.104(3) Uani 1 1 d . . . H58 H 0.0423 -0.3532 0.4597 0.125 Uiso 1 1 calc R . . C9 C 0.2747(6) -0.4184(3) 0.2021(5) 0.087(2) Uani 1 1 d . . . H9 H 0.2639 -0.4475 0.1764 0.104 Uiso 1 1 calc R . . C57 C 0.1207(6) -0.3009(3) 0.5154(5) 0.093(3) Uani 1 1 d . . . H57 H 0.1153 -0.3147 0.5585 0.112 Uiso 1 1 calc R . . C11 C 0.2625(6) -0.3725(3) 0.3031(4) 0.088(2) Uani 1 1 d . . . H11 H 0.2433 -0.3701 0.3467 0.105 Uiso 1 1 calc R . . C59 C 0.0872(8) -0.3034(3) 0.3952(5) 0.131(4) Uani 1 1 d . . . H59 H 0.0575 -0.3188 0.3545 0.158 Uiso 1 1 calc R . . C8 C 0.3179(5) -0.3784(2) 0.1748(4) 0.069(2) Uani 1 1 d . . . H8 H 0.3354 -0.3807 0.1307 0.082 Uiso 1 1 calc R . . C56 C 0.1733(5) -0.2569(3) 0.5123(4) 0.077(2) Uani 1 1 d . . . H56 H 0.2021 -0.2415 0.5533 0.092 Uiso 1 1 calc R . . C12 C 0.3058(5) -0.3322(3) 0.2759(4) 0.070(2) Uani 1 1 d . . . H12 H 0.3147 -0.3029 0.3013 0.084 Uiso 1 1 calc R . . C5 C 0.6665(6) -0.3522(3) 0.2303(6) 0.150(5) Uani 1 1 d . . . H5 H 0.6890 -0.3838 0.2444 0.180 Uiso 1 1 calc R . . C7 C 0.3359(4) -0.3347(2) 0.2120(3) 0.0463(15) Uani 1 1 d . . . C60 C 0.1402(7) -0.2600(3) 0.3914(4) 0.109(3) Uani 1 1 d . . . H60 H 0.1465 -0.2471 0.3480 0.130 Uiso 1 1 calc R . . C6 C 0.5652(5) -0.3431(3) 0.2154(5) 0.104(3) Uani 1 1 d . . . H6 H 0.5205 -0.3689 0.2187 0.125 Uiso 1 1 calc R . . C55 C 0.1835(5) -0.2357(2) 0.4501(4) 0.0556(17) Uani 1 1 d . . . C69 C 0.4825(7) -0.2121(5) 0.5872(6) 0.124(4) Uani 1 1 d . . . H69 H 0.5185 -0.2408 0.6005 0.149 Uiso 1 1 calc R . . C68 C 0.4016(6) -0.2147(3) 0.5353(4) 0.089(2) Uani 1 1 d . . . H68 H 0.3841 -0.2451 0.5145 0.107 Uiso 1 1 calc R . . C4 C 0.7343(6) -0.3152(3) 0.2247(5) 0.113(3) Uani 1 1 d . . . H4 H 0.8026 -0.3216 0.2334 0.135 Uiso 1 1 calc R . . C70 C 0.5104(8) -0.1698(6) 0.6186(6) 0.141(5) Uani 1 1 d . . . H70 H 0.5640 -0.1687 0.6548 0.169 Uiso 1 1 calc R . . C1 C 0.5291(4) -0.2973(2) 0.1962(3) 0.0461(15) Uani 1 1 d . . . C67 C 0.3465(5) -0.1740(3) 0.5135(3) 0.0570(17) Uani 1 1 d . . . C66 C 0.1303(6) -0.1291(3) 0.5325(5) 0.102(3) Uani 1 1 d . . . H66 H 0.1676 -0.1476 0.5676 0.122 Uiso 1 1 calc R . . C13 C 0.3581(4) -0.2854(2) 0.0863(3) 0.0456(15) Uani 1 1 d . . . C18 C 0.2581(5) -0.2834(3) 0.0608(4) 0.087(2) Uani 1 1 d . . . H18 H 0.2128 -0.2815 0.0921 0.104 Uiso 1 1 calc R . . C3 C 0.7001(5) -0.2698(3) 0.2065(4) 0.082(2) Uani 1 1 d . . . H3 H 0.7450 -0.2441 0.2033 0.099 Uiso 1 1 calc R . . C71 C 0.4586(9) -0.1276(5) 0.5967(5) 0.135(4) Uani 1 1 d . . . H71 H 0.4778 -0.0975 0.6181 0.162 Uiso 1 1 calc R . . C65 C 0.0540(8) -0.0984(4) 0.5478(6) 0.140(5) Uani 1 1 d . . . H65 H 0.0386 -0.0973 0.5926 0.168 Uiso 1 1 calc R . . C17 C 0.2222(6) -0.2840(3) -0.0086(5) 0.097(3) Uani 1 1 d . . . H17 H 0.1535 -0.2838 -0.0238 0.116 Uiso 1 1 calc R . . C14 C 0.4219(6) -0.2866(3) 0.0394(4) 0.093(3) Uani 1 1 d . . . H14 H 0.4905 -0.2877 0.0546 0.112 Uiso 1 1 calc R . . C2 C 0.5983(5) -0.2608(2) 0.1924(3) 0.0647(19) Uani 1 1 d . . . H2 H 0.5763 -0.2289 0.1800 0.078 Uiso 1 1 calc R . . C72 C 0.3780(6) -0.1289(3) 0.5430(4) 0.098(3) Uani 1 1 d . . . H72 H 0.3455 -0.0997 0.5271 0.118 Uiso 1 1 calc R . . C61 C 0.1510(5) -0.1323(2) 0.4649(4) 0.0613(19) Uani 1 1 d . . . C15 C 0.3859(7) -0.2862(4) -0.0310(4) 0.123(4) Uani 1 1 d . . . H15 H 0.4312 -0.2869 -0.0623 0.148 Uiso 1 1 calc R . . C16 C 0.2863(8) -0.2849(3) -0.0558(4) 0.095(3) Uani 1 1 d . . . H16 H 0.2629 -0.2846 -0.1033 0.114 Uiso 1 1 calc R . . C64 C 0.0020(7) -0.0699(4) 0.4965(8) 0.125(4) Uani 1 1 d . . . H64 H -0.0488 -0.0491 0.5062 0.150 Uiso 1 1 calc R . . C62 C 0.0998(5) -0.1027(3) 0.4159(4) 0.082(2) Uani 1 1 d . . . H62 H 0.1154 -0.1031 0.3711 0.098 Uiso 1 1 calc R . . C63 C 0.0250(6) -0.0720(3) 0.4312(5) 0.102(3) Uani 1 1 d . . . H63 H -0.0102 -0.0525 0.3963 0.122 Uiso 1 1 calc R . . C33 C 0.8774(5) -0.1465(2) 0.2864(4) 0.072(2) Uani 1 1 d . . . H33 H 0.9306 -0.1577 0.3188 0.086 Uiso 1 1 calc R . . C23 C 0.6532(8) -0.0624(4) 0.4978(4) 0.147(5) Uani 1 1 d . . . H23 H 0.6291 -0.0794 0.5333 0.176 Uiso 1 1 calc R . . C52 C -0.0107(9) -0.1649(4) -0.0488(5) 0.115(4) Uani 1 1 d . . . H52 H -0.0471 -0.1857 -0.0815 0.138 Uiso 1 1 calc R . . C34 C 0.8763(5) -0.1572(2) 0.2176(5) 0.072(2) Uani 1 1 d . . . H34 H 0.9288 -0.1746 0.2032 0.087 Uiso 1 1 calc R . . C24 C 0.6224(6) -0.0758(3) 0.4291(4) 0.109(3) Uani 1 1 d . . . H24 H 0.5769 -0.1016 0.4186 0.131 Uiso 1 1 calc R . . C51 C -0.0602(7) -0.1355(3) -0.0090(5) 0.100(3) Uani 1 1 d . . . H51 H -0.1296 -0.1361 -0.0146 0.120 Uiso 1 1 calc R . . C53 C 0.0914(9) -0.1646(3) -0.0420(5) 0.125(4) Uani 1 1 d . . . H53 H 0.1248 -0.1844 -0.0700 0.149 Uiso 1 1 calc R . . C32 C 0.8024(4) -0.1199(2) 0.3089(4) 0.0604(18) Uani 1 1 d . . . H32 H 0.8061 -0.1126 0.3559 0.073 Uiso 1 1 calc R . . C35 C 0.7959(5) -0.1417(2) 0.1698(4) 0.0670(19) Uani 1 1 d . . . H35 H 0.7939 -0.1486 0.1228 0.080 Uiso 1 1 calc R . . C54 C 0.1438(6) -0.1336(3) 0.0083(4) 0.101(3) Uani 1 1 d . . . H54 H 0.2133 -0.1338 0.0146 0.121 Uiso 1 1 calc R . . C22 C 0.7191(7) -0.0240(4) 0.5132(5) 0.110(3) Uani 1 1 d . . . H22 H 0.7400 -0.0150 0.5592 0.132 Uiso 1 1 calc R . . C31 C 0.7198(4) -0.1035(2) 0.2614(3) 0.0454(15) Uani 1 1 d . . . C50 C -0.0064(5) -0.1046(3) 0.0401(4) 0.077(2) Uani 1 1 d . . . H50 H -0.0407 -0.0848 0.0676 0.093 Uiso 1 1 calc R . . C36 C 0.7181(5) -0.1158(2) 0.1918(3) 0.0570(17) Uani 1 1 d . . . H36 H 0.6635 -0.1064 0.1594 0.068 Uiso 1 1 calc R . . C49 C 0.0953(5) -0.1025(2) 0.0493(3) 0.0578(17) Uani 1 1 d . . . C19 C 0.6584(4) -0.0514(2) 0.3770(3) 0.0489(16) Uani 1 1 d . . . C42 C 0.0371(5) -0.0484(3) 0.2025(4) 0.068(2) Uani 1 1 d . . . H42 H 0.0533 -0.0808 0.2161 0.081 Uiso 1 1 calc R . . C41 C -0.0315(5) -0.0225(3) 0.2347(4) 0.080(2) Uani 1 1 d . . . H41 H -0.0617 -0.0375 0.2691 0.096 Uiso 1 1 calc R . . C21 C 0.7541(6) 0.0008(3) 0.4621(5) 0.092(3) Uani 1 1 d . . . H21 H 0.7987 0.0269 0.4724 0.110 Uiso 1 1 calc R . . C20 C 0.7229(5) -0.0132(2) 0.3945(4) 0.070(2) Uani 1 1 d . . . H20 H 0.7468 0.0042 0.3592 0.084 Uiso 1 1 calc R . . C37 C 0.0814(4) -0.0272(2) 0.1512(3) 0.0473(15) Uani 1 1 d . . . C40 C -0.0540(5) 0.0254(3) 0.2151(4) 0.071(2) Uani 1 1 d . . . H40 H -0.0989 0.0434 0.2369 0.085 Uiso 1 1 calc R . . C25 C 0.6101(4) -0.0114(2) 0.2413(3) 0.0440(15) Uani 1 1 d . . . C43 C 0.2333(4) -0.0220(2) 0.0635(3) 0.0477(15) Uani 1 1 d . . . C38 C 0.0566(4) 0.0209(2) 0.1323(3) 0.0557(17) Uani 1 1 d . . . H38 H 0.0861 0.0359 0.0977 0.067 Uiso 1 1 calc R . . C39 C -0.0114(5) 0.0472(2) 0.1639(4) 0.071(2) Uani 1 1 d . . . H39 H -0.0280 0.0796 0.1503 0.086 Uiso 1 1 calc R . . C30 C 0.5367(5) 0.0219(2) 0.2512(3) 0.0644(19) Uani 1 1 d . . . H30 H 0.4902 0.0130 0.2795 0.077 Uiso 1 1 calc R . . C44 C 0.3299(5) -0.0059(2) 0.0888(3) 0.0627(18) Uani 1 1 d . . . H44 H 0.3610 -0.0167 0.1322 0.075 Uiso 1 1 calc R . . C26 C 0.6779(4) 0.0034(2) 0.1999(3) 0.0608(18) Uani 1 1 d . . . H26 H 0.7294 -0.0179 0.1930 0.073 Uiso 1 1 calc R . . C48 C 0.1891(5) -0.0042(3) -0.0015(3) 0.0661(19) Uani 1 1 d . . . H48 H 0.1249 -0.0144 -0.0200 0.079 Uiso 1 1 calc R . . C45 C 0.3802(5) 0.0260(3) 0.0509(4) 0.080(2) Uani 1 1 d . . . H45 H 0.4452 0.0358 0.0680 0.096 Uiso 1 1 calc R . . C29 C 0.5300(5) 0.0678(3) 0.2206(4) 0.076(2) Uani 1 1 d . . . H29 H 0.4792 0.0894 0.2282 0.092 Uiso 1 1 calc R . . C27 C 0.6709(6) 0.0498(3) 0.1681(4) 0.076(2) Uani 1 1 d . . . H27 H 0.7165 0.0587 0.1392 0.091 Uiso 1 1 calc R . . C47 C 0.2387(6) 0.0282(3) -0.0384(4) 0.080(2) Uani 1 1 d . . . H47 H 0.2077 0.0400 -0.0813 0.096 Uiso 1 1 calc R . . C46 C 0.3333(7) 0.0430(3) -0.0125(4) 0.088(2) Uani 1 1 d . . . H46 H 0.3666 0.0649 -0.0379 0.106 Uiso 1 1 calc R . . C28 C 0.5979(5) 0.0823(2) 0.1789(4) 0.0671(19) Uani 1 1 d . . . H28 H 0.5940 0.1136 0.1584 0.081 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 I4 0.0439(2) 0.0466(2) 0.0442(2) 0.00421(18) -0.00217(18) 0.00206(19) I3 0.0381(2) 0.0513(3) 0.0644(3) 0.0003(2) -0.00066(19) -0.0039(2) I2 0.0488(2) 0.0487(2) 0.0443(2) 0.00032(19) 0.00628(18) 0.0058(2) I1 0.0527(3) 0.0377(2) 0.0580(3) -0.00438(19) 0.0130(2) 0.0012(2) Cu1 0.0541(5) 0.0474(5) 0.0590(5) -0.0095(4) 0.0019(4) 0.0044(4) Cu4 0.0587(5) 0.0552(5) 0.0621(5) 0.0031(4) 0.0151(4) -0.0021(4) Cu2 0.0444(5) 0.0520(5) 0.0590(5) -0.0031(4) 0.0057(4) -0.0074(4) Cu3 0.0501(5) 0.0577(5) 0.0573(5) 0.0076(4) 0.0003(4) 0.0113(4) P1 0.0410(9) 0.0386(9) 0.0471(10) -0.0038(7) 0.0025(7) -0.0006(7) P4 0.0504(10) 0.0437(10) 0.0616(12) -0.0007(8) 0.0189(8) -0.0001(8) P2 0.0404(9) 0.0439(9) 0.0441(10) -0.0016(7) 0.0056(7) -0.0049(8) P3 0.0453(10) 0.0466(10) 0.0479(10) 0.0028(8) -0.0009(8) 0.0073(8) C10 0.071(5) 0.075(6) 0.117(8) 0.035(6) 0.013(5) -0.024(5) C58 0.144(9) 0.065(6) 0.113(8) 0.000(6) 0.046(7) -0.045(6) C9 0.099(6) 0.063(5) 0.098(7) -0.009(5) 0.010(5) -0.025(5) C57 0.110(7) 0.086(6) 0.089(7) 0.026(5) 0.030(5) -0.032(5) C11 0.090(6) 0.102(7) 0.076(6) 0.027(5) 0.028(5) -0.013(5) C59 0.212(11) 0.091(7) 0.103(8) -0.020(6) 0.060(7) -0.080(7) C8 0.084(5) 0.054(4) 0.071(5) -0.006(4) 0.020(4) -0.025(4) C56 0.084(5) 0.072(5) 0.076(6) 0.012(4) 0.019(4) -0.017(4) C12 0.078(5) 0.059(5) 0.075(5) 0.004(4) 0.020(4) -0.014(4) C5 0.052(5) 0.090(7) 0.295(14) 0.102(8) -0.010(7) 0.008(5) C7 0.038(3) 0.045(4) 0.058(4) 0.000(3) 0.013(3) -0.002(3) C60 0.190(9) 0.075(6) 0.072(6) -0.013(5) 0.057(6) -0.064(6) C6 0.045(5) 0.068(5) 0.192(9) 0.057(6) -0.002(5) -0.009(4) C55 0.068(4) 0.043(4) 0.061(5) 0.001(3) 0.028(4) -0.002(3) C69 0.065(7) 0.179(13) 0.125(10) 0.026(8) 0.000(6) 0.028(7) C68 0.058(5) 0.094(6) 0.115(7) 0.006(5) 0.008(5) 0.014(5) C4 0.047(5) 0.099(7) 0.185(10) 0.056(7) -0.005(5) -0.001(5) C70 0.071(7) 0.258(19) 0.090(9) -0.021(10) 0.000(6) 0.003(10) C1 0.049(4) 0.039(4) 0.050(4) 0.004(3) 0.004(3) 0.003(3) C67 0.051(4) 0.071(5) 0.054(4) 0.000(4) 0.024(3) 0.002(4) C66 0.123(7) 0.073(5) 0.129(8) 0.038(5) 0.079(6) 0.035(5) C13 0.044(4) 0.036(3) 0.056(4) -0.009(3) 0.004(3) 0.002(3) C18 0.063(5) 0.136(8) 0.060(5) -0.019(5) 0.000(4) 0.006(5) C3 0.046(5) 0.078(6) 0.119(7) 0.031(5) 0.002(4) -0.013(4) C71 0.127(10) 0.175(13) 0.094(9) -0.049(8) -0.009(7) -0.034(8) C65 0.164(10) 0.091(7) 0.198(12) 0.014(7) 0.136(10) 0.042(7) C17 0.070(6) 0.128(8) 0.081(7) -0.015(6) -0.026(5) 0.011(5) C14 0.067(5) 0.160(8) 0.052(5) -0.021(5) 0.005(4) 0.006(5) C2 0.053(4) 0.048(4) 0.090(5) 0.011(4) 0.003(4) -0.005(4) C72 0.107(7) 0.095(7) 0.090(7) -0.015(5) 0.003(5) -0.009(5) C61 0.058(4) 0.037(4) 0.095(6) -0.003(4) 0.031(4) -0.004(3) C15 0.098(7) 0.219(12) 0.054(6) -0.027(6) 0.016(5) -0.005(7) C16 0.123(8) 0.098(7) 0.057(6) -0.006(5) -0.006(6) 0.009(6) C64 0.083(7) 0.070(7) 0.239(15) -0.027(8) 0.072(9) 0.002(5) C62 0.058(5) 0.078(6) 0.104(7) -0.019(5) -0.002(4) 0.014(4) C63 0.059(6) 0.096(7) 0.140(9) -0.026(6) -0.019(5) 0.018(5) C33 0.047(4) 0.065(5) 0.098(7) 0.001(4) -0.003(4) 0.016(4) C23 0.194(11) 0.196(12) 0.049(6) -0.016(6) 0.014(6) -0.097(9) C52 0.148(10) 0.081(7) 0.099(8) -0.011(6) -0.037(7) -0.017(7) C34 0.048(5) 0.062(5) 0.109(7) -0.023(5) 0.020(5) -0.004(4) C24 0.150(8) 0.124(7) 0.055(6) -0.016(5) 0.019(5) -0.079(6) C51 0.097(7) 0.096(7) 0.098(7) -0.014(6) -0.014(6) -0.028(6) C53 0.172(10) 0.073(6) 0.107(8) -0.038(5) -0.047(7) 0.037(7) C32 0.043(4) 0.062(4) 0.072(5) 0.000(4) -0.001(4) -0.004(4) C35 0.062(5) 0.074(5) 0.070(5) -0.014(4) 0.026(4) -0.011(4) C54 0.105(7) 0.098(7) 0.087(6) -0.026(5) -0.025(5) 0.039(6) C22 0.138(9) 0.117(8) 0.067(7) -0.040(6) -0.008(6) -0.021(7) C31 0.037(4) 0.047(4) 0.050(4) -0.003(3) 0.002(3) -0.011(3) C50 0.070(5) 0.085(6) 0.070(5) -0.007(4) -0.007(4) -0.015(5) C36 0.050(4) 0.063(4) 0.059(5) -0.001(3) 0.012(3) -0.002(4) C49 0.064(5) 0.041(4) 0.062(5) 0.006(3) -0.009(4) 0.005(4) C19 0.050(4) 0.039(4) 0.055(4) -0.004(3) 0.002(3) -0.007(3) C42 0.056(4) 0.064(5) 0.087(6) 0.018(4) 0.020(4) 0.010(4) C41 0.067(5) 0.080(6) 0.103(6) 0.018(5) 0.040(4) 0.007(5) C21 0.103(7) 0.060(5) 0.096(7) -0.018(5) -0.035(6) -0.007(5) C20 0.075(5) 0.060(5) 0.068(5) -0.004(4) -0.009(4) -0.015(4) C37 0.044(4) 0.044(4) 0.051(4) 0.005(3) -0.003(3) -0.003(3) C40 0.054(5) 0.068(5) 0.096(6) -0.021(4) 0.023(4) 0.008(4) C25 0.038(3) 0.044(4) 0.048(4) -0.003(3) 0.004(3) -0.004(3) C43 0.047(4) 0.046(4) 0.050(4) -0.001(3) 0.007(3) 0.008(3) C38 0.061(4) 0.049(4) 0.056(4) 0.010(3) 0.006(3) 0.006(4) C39 0.068(5) 0.047(4) 0.099(6) -0.005(4) 0.011(4) 0.018(4) C30 0.059(5) 0.050(4) 0.085(5) 0.015(4) 0.016(4) 0.002(4) C44 0.074(5) 0.053(4) 0.060(5) 0.000(3) 0.009(4) -0.006(4) C26 0.053(4) 0.054(4) 0.079(5) 0.012(4) 0.023(4) 0.005(3) C48 0.065(5) 0.079(5) 0.052(5) 0.014(4) 0.002(4) 0.001(4) C45 0.068(5) 0.075(5) 0.094(7) 0.006(5) 0.002(5) -0.020(4) C29 0.059(5) 0.064(5) 0.107(6) -0.004(5) 0.015(4) 0.016(4) C27 0.082(5) 0.067(5) 0.083(6) 0.020(4) 0.023(4) -0.007(5) C47 0.097(6) 0.095(6) 0.047(5) 0.020(4) 0.005(4) -0.001(5) C46 0.111(7) 0.089(6) 0.067(6) 0.015(5) 0.021(5) -0.017(6) C28 0.068(5) 0.046(4) 0.082(5) 0.013(4) -0.002(4) -0.003(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 I4 Cu1 2.6620(8) . ? I4 Cu4 2.6909(9) . ? I4 Cu2 2.7078(8) . ? I4 I1 4.2361(6) . ? I4 I2 4.3897(6) . ? I4 I3 4.4858(6) . ? I3 Cu1 2.6547(9) . ? I3 Cu3 2.6973(9) . ? I3 Cu4 2.7195(9) . ? I3 I1 4.2715(6) . ? I3 I2 4.3555(6) . ? I2 Cu3 2.6704(9) . ? I2 Cu2 2.6892(9) . ? I2 Cu1 2.7353(9) . ? I2 I1 4.5023(6) . ? I1 Cu3 2.6700(9) . ? I1 Cu2 2.7057(8) . ? I1 Cu4 2.7141(9) . ? Cu1 P1 2.2531(16) . ? Cu1 Cu4 2.8676(11) . ? Cu1 Cu3 2.8971(10) . ? Cu1 Cu2 2.9277(10) . ? Cu4 P4 2.2608(18) . ? Cu4 Cu3 3.1084(11) . ? Cu4 Cu2 3.1658(10) . ? Cu2 P2 2.2579(16) . ? Cu2 Cu3 2.8400(10) . ? Cu3 P3 2.2518(17) . ? P1 C13 1.808(6) . ? P1 C7 1.810(6) . ? P1 C1 1.828(6) . ? P4 C67 1.820(7) . ? P4 C55 1.827(6) . ? P4 C61 1.835(6) . ? P2 C31 1.821(6) . ? P2 C25 1.825(6) . ? P2 C19 1.827(6) . ? P3 C43 1.808(6) . ? P3 C49 1.817(6) . ? P3 C37 1.827(6) . ? C10 C11 1.365(10) . ? C10 C9 1.369(10) . ? C58 C57 1.338(10) . ? C58 C59 1.357(10) . ? C9 C8 1.371(9) . ? C57 C56 1.391(9) . ? C11 C12 1.378(9) . ? C59 C60 1.379(10) . ? C8 C7 1.384(8) . ? C56 C55 1.366(8) . ? C12 C7 1.372(8) . ? C5 C4 1.372(10) . ? C5 C6 1.379(9) . ? C60 C55 1.369(9) . ? C6 C1 1.358(8) . ? C69 C70 1.323(14) . ? C69 C68 1.370(11) . ? C68 C67 1.355(9) . ? C4 C3 1.335(9) . ? C70 C71 1.368(14) . ? C1 C2 1.369(7) . ? C67 C72 1.384(9) . ? C66 C65 1.391(10) . ? C66 C61 1.392(9) . ? C13 C14 1.353(8) . ? C13 C18 1.369(8) . ? C18 C17 1.365(9) . ? C3 C2 1.384(8) . ? C71 C72 1.388(11) . ? C65 C64 1.367(13) . ? C17 C16 1.360(10) . ? C14 C15 1.381(10) . ? C61 C62 1.348(9) . ? C15 C16 1.361(10) . ? C64 C63 1.357(12) . ? C62 C63 1.376(10) . ? C33 C34 1.370(9) . ? C33 C32 1.371(8) . ? C23 C22 1.369(11) . ? C23 C24 1.386(10) . ? C52 C51 1.356(11) . ? C52 C53 1.368(12) . ? C34 C35 1.382(9) . ? C24 C19 1.364(9) . ? C51 C50 1.386(9) . ? C53 C54 1.392(10) . ? C32 C31 1.406(8) . ? C35 C36 1.387(8) . ? C54 C49 1.393(9) . ? C22 C21 1.345(10) . ? C31 C36 1.391(8) . ? C50 C49 1.361(8) . ? C19 C20 1.359(8) . ? C42 C37 1.369(8) . ? C42 C41 1.388(8) . ? C41 C40 1.368(9) . ? C21 C20 1.371(9) . ? C37 C38 1.374(7) . ? C40 C39 1.360(9) . ? C25 C26 1.373(7) . ? C25 C30 1.374(8) . ? C43 C44 1.393(8) . ? C43 C48 1.398(8) . ? C38 C39 1.382(8) . ? C30 C29 1.371(8) . ? C44 C45 1.380(8) . ? C26 C27 1.392(8) . ? C48 C47 1.371(8) . ? C45 C46 1.375(9) . ? C29 C28 1.376(9) . ? C27 C28 1.361(9) . ? C47 C46 1.361(9) . ? 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 Cu1 I4 Cu4 64.78(2) . . ? Cu1 I4 Cu2 66.07(2) . . ? Cu4 I4 Cu2 71.80(2) . . ? Cu1 I4 I1 74.178(18) . . ? Cu4 I4 I1 38.590(18) . . ? Cu2 I4 I1 38.492(17) . . ? Cu1 I4 I2 36.139(18) . . ? Cu4 I4 I2 78.437(19) . . ? Cu2 I4 I2 35.433(17) . . ? I1 I4 I2 62.896(9) . . ? Cu1 I4 I3 32.415(18) . . ? Cu4 I4 I3 34.198(19) . . ? Cu2 I4 I3 72.947(18) . . ? I1 I4 I3 58.564(9) . . ? I2 I4 I3 58.766(9) . . ? Cu1 I3 Cu3 65.54(2) . . ? Cu1 I3 Cu4 64.48(2) . . ? Cu3 I3 Cu4 70.04(2) . . ? Cu1 I3 I1 73.580(18) . . ? Cu3 I3 I1 37.043(18) . . ? Cu4 I3 I1 38.129(18) . . ? Cu1 I3 I2 36.720(18) . . ? Cu3 I3 I2 35.557(18) . . ? Cu4 I3 I2 78.825(19) . . ? I1 I3 I2 62.908(9) . . ? Cu1 I3 I4 32.516(18) . . ? Cu3 I3 I4 71.580(18) . . ? Cu4 I3 I4 33.790(18) . . ? I1 I3 I4 57.796(9) . . ? I2 I3 I4 59.516(10) . . ? Cu3 I2 Cu2 64.00(2) . . ? Cu3 I2 Cu1 64.80(2) . . ? Cu2 I2 Cu1 65.32(2) . . ? Cu3 I2 I3 35.971(18) . . ? Cu2 I2 I3 75.482(18) . . ? Cu1 I2 I3 35.470(17) . . ? Cu3 I2 I4 73.523(19) . . ? Cu2 I2 I4 35.716(17) . . ? Cu1 I2 I4 35.026(17) . . ? I3 I2 I4 61.718(9) . . ? Cu3 I2 I1 32.532(18) . . ? Cu2 I2 I1 33.548(17) . . ? Cu1 I2 I1 68.892(18) . . ? I3 I2 I1 57.634(9) . . ? I4 I2 I1 56.884(9) . . ? Cu3 I1 Cu2 63.78(2) . . ? Cu3 I1 Cu4 70.52(3) . . ? Cu2 I1 Cu4 71.48(2) . . ? Cu3 I1 I4 76.392(18) . . ? Cu2 I1 I4 38.527(17) . . ? Cu4 I1 I4 38.200(18) . . ? Cu3 I1 I3 37.488(18) . . ? Cu2 I1 I3 76.907(18) . . ? Cu4 I1 I3 38.220(19) . . ? I4 I1 I3 63.640(10) . . ? Cu3 I1 I2 32.538(18) . . ? Cu2 I1 I2 33.317(17) . . ? Cu4 I1 I2 76.123(19) . . ? I4 I1 I2 60.220(9) . . ? I3 I1 I2 59.458(9) . . ? P1 Cu1 I3 111.90(5) . . ? P1 Cu1 I4 106.57(5) . . ? I3 Cu1 I4 115.07(3) . . ? P1 Cu1 I2 106.29(5) . . ? I3 Cu1 I2 107.81(3) . . ? I4 Cu1 I2 108.83(3) . . ? P1 Cu1 Cu4 140.83(5) . . ? I3 Cu1 Cu4 58.85(2) . . ? I4 Cu1 Cu4 58.10(2) . . ? I2 Cu1 Cu4 112.77(3) . . ? P1 Cu1 Cu3 146.77(5) . . ? I3 Cu1 Cu3 57.94(2) . . ? I4 Cu1 Cu3 106.08(3) . . ? I2 Cu1 Cu3 56.52(2) . . ? Cu4 Cu1 Cu3 65.26(3) . . ? P1 Cu1 Cu2 140.28(5) . . ? I3 Cu1 Cu2 107.64(3) . . ? I4 Cu1 Cu2 57.72(2) . . ? I2 Cu1 Cu2 56.58(2) . . ? Cu4 Cu1 Cu2 66.21(3) . . ? Cu3 Cu1 Cu2 58.36(3) . . ? P4 Cu4 I4 107.24(5) . . ? P4 Cu4 I1 112.94(5) . . ? I4 Cu4 I1 103.21(3) . . ? P4 Cu4 I3 117.00(5) . . ? I4 Cu4 I3 112.01(3) . . ? I1 Cu4 I3 103.65(3) . . ? P4 Cu4 Cu1 144.38(5) . . ? I4 Cu4 Cu1 57.12(2) . . ? I1 Cu4 Cu1 102.21(3) . . ? I3 Cu4 Cu1 56.66(2) . . ? P4 Cu4 Cu3 152.45(5) . . ? I4 Cu4 Cu3 99.80(3) . . ? I1 Cu4 Cu3 54.08(2) . . ? I3 Cu4 Cu3 54.65(2) . . ? Cu1 Cu4 Cu3 57.83(3) . . ? P4 Cu4 Cu2 143.26(5) . . ? I4 Cu4 Cu2 54.35(2) . . ? I1 Cu4 Cu2 54.14(2) . . ? I3 Cu4 Cu2 99.74(3) . . ? Cu1 Cu4 Cu2 57.80(2) . . ? Cu3 Cu4 Cu2 53.82(2) . . ? P2 Cu2 I2 108.78(5) . . ? P2 Cu2 I1 110.03(5) . . ? I2 Cu2 I1 113.13(3) . . ? P2 Cu2 I4 113.05(5) . . ? I2 Cu2 I4 108.85(3) . . ? I1 Cu2 I4 102.98(3) . . ? P2 Cu2 Cu3 140.47(5) . . ? I2 Cu2 Cu3 57.68(2) . . ? I1 Cu2 Cu3 57.50(2) . . ? I4 Cu2 Cu3 106.44(3) . . ? P2 Cu2 Cu1 149.05(5) . . ? I2 Cu2 Cu1 58.10(2) . . ? I1 Cu2 Cu1 100.88(3) . . ? I4 Cu2 Cu1 56.21(2) . . ? Cu3 Cu2 Cu1 60.28(3) . . ? P2 Cu2 Cu4 145.82(5) . . ? I2 Cu2 Cu4 105.40(3) . . ? I1 Cu2 Cu4 54.38(2) . . ? I4 Cu2 Cu4 53.85(2) . . ? Cu3 Cu2 Cu4 62.06(3) . . ? Cu1 Cu2 Cu4 55.98(2) . . ? P3 Cu3 I1 113.05(5) . . ? P3 Cu3 I2 107.32(5) . . ? I1 Cu3 I2 114.93(3) . . ? P3 Cu3 I3 107.28(5) . . ? I1 Cu3 I3 105.47(3) . . ? I2 Cu3 I3 108.47(3) . . ? P3 Cu3 Cu2 143.64(5) . . ? I1 Cu3 Cu2 58.72(2) . . ? I2 Cu3 Cu2 58.32(2) . . ? I3 Cu3 Cu2 109.00(3) . . ? P3 Cu3 Cu1 144.11(5) . . ? I1 Cu3 Cu1 102.55(3) . . ? I2 Cu3 Cu1 58.68(2) . . ? I3 Cu3 Cu1 56.52(2) . . ? Cu2 Cu3 Cu1 61.36(3) . . ? P3 Cu3 Cu4 144.72(5) . . ? I1 Cu3 Cu4 55.40(2) . . ? I2 Cu3 Cu4 107.46(3) . . ? I3 Cu3 Cu4 55.32(2) . . ? Cu2 Cu3 Cu4 64.12(3) . . ? Cu1 Cu3 Cu4 56.91(2) . . ? C13 P1 C7 103.6(3) . . ? C13 P1 C1 106.5(3) . . ? C7 P1 C1 103.9(3) . . ? C13 P1 Cu1 112.17(18) . . ? C7 P1 Cu1 117.8(2) . . ? C1 P1 Cu1 111.89(19) . . ? C67 P4 C55 104.4(3) . . ? C67 P4 C61 104.8(3) . . ? C55 P4 C61 101.9(3) . . ? C67 P4 Cu4 112.42(19) . . ? C55 P4 Cu4 116.6(2) . . ? C61 P4 Cu4 115.4(3) . . ? C31 P2 C25 104.8(3) . . ? C31 P2 C19 104.5(3) . . ? C25 P2 C19 101.8(3) . . ? C31 P2 Cu2 113.05(18) . . ? C25 P2 Cu2 114.99(18) . . ? C19 P2 Cu2 116.2(2) . . ? C43 P3 C49 103.5(3) . . ? C43 P3 C37 104.6(3) . . ? C49 P3 C37 103.7(3) . . ? C43 P3 Cu3 115.7(2) . . ? C49 P3 Cu3 113.7(2) . . ? C37 P3 Cu3 114.15(19) . . ? C11 C10 C9 118.7(7) . . ? C57 C58 C59 118.5(8) . . ? C10 C9 C8 120.7(7) . . ? C58 C57 C56 121.0(8) . . ? C10 C11 C12 120.8(8) . . ? C58 C59 C60 121.1(9) . . ? C9 C8 C7 121.1(7) . . ? C55 C56 C57 121.3(7) . . ? C7 C12 C11 121.0(7) . . ? C4 C5 C6 120.6(7) . . ? C12 C7 C8 117.6(6) . . ? C12 C7 P1 119.7(5) . . ? C8 C7 P1 122.8(5) . . ? C55 C60 C59 121.3(7) . . ? C1 C6 C5 121.6(7) . . ? C56 C55 C60 116.9(6) . . ? C56 C55 P4 124.3(6) . . ? C60 C55 P4 118.8(5) . . ? C70 C69 C68 121.4(12) . . ? C67 C68 C69 121.9(9) . . ? C3 C4 C5 118.6(7) . . ? C69 C70 C71 118.5(12) . . ? C6 C1 C2 116.6(6) . . ? C6 C1 P1 124.1(5) . . ? C2 C1 P1 119.2(5) . . ? C68 C67 C72 117.5(7) . . ? C68 C67 P4 122.4(6) . . ? C72 C67 P4 119.7(6) . . ? C65 C66 C61 120.4(8) . . ? C14 C13 C18 117.1(6) . . ? C14 C13 P1 124.6(5) . . ? C18 C13 P1 118.1(5) . . ? C17 C18 C13 122.6(7) . . ? C4 C3 C2 120.5(7) . . ? C70 C71 C72 121.2(11) . . ? C64 C65 C66 119.5(10) . . ? C16 C17 C18 120.3(8) . . ? C13 C14 C15 120.5(7) . . ? C1 C2 C3 122.1(6) . . ? C67 C72 C71 119.3(9) . . ? C62 C61 C66 118.4(7) . . ? C62 C61 P4 119.8(6) . . ? C66 C61 P4 121.8(6) . . ? C16 C15 C14 121.9(8) . . ? C17 C16 C15 117.5(8) . . ? C63 C64 C65 119.6(10) . . ? C61 C62 C63 121.1(8) . . ? C64 C63 C62 120.9(9) . . ? C34 C33 C32 121.9(7) . . ? C22 C23 C24 119.7(8) . . ? C51 C52 C53 121.6(9) . . ? C33 C34 C35 118.8(7) . . ? C19 C24 C23 120.3(7) . . ? C52 C51 C50 119.5(9) . . ? C52 C53 C54 117.8(9) . . ? C33 C32 C31 120.4(7) . . ? C34 C35 C36 120.0(7) . . ? C53 C54 C49 122.1(8) . . ? C21 C22 C23 120.4(8) . . ? C36 C31 C32 117.2(6) . . ? C36 C31 P2 119.5(5) . . ? C32 C31 P2 123.1(5) . . ? C49 C50 C51 121.8(8) . . ? C35 C36 C31 121.6(6) . . ? C50 C49 C54 117.2(7) . . ? C50 C49 P3 124.9(6) . . ? C54 C49 P3 117.8(6) . . ? C20 C19 C24 118.0(6) . . ? C20 C19 P2 123.6(5) . . ? C24 C19 P2 118.3(5) . . ? C37 C42 C41 121.5(6) . . ? C40 C41 C42 118.9(7) . . ? C22 C21 C20 119.0(8) . . ? C19 C20 C21 122.5(7) . . ? C42 C37 C38 118.2(6) . . ? C42 C37 P3 116.9(5) . . ? C38 C37 P3 124.9(5) . . ? C39 C40 C41 120.7(6) . . ? C26 C25 C30 117.2(6) . . ? C26 C25 P2 124.8(5) . . ? C30 C25 P2 117.9(5) . . ? C44 C43 C48 117.3(6) . . ? C44 C43 P3 119.4(5) . . ? C48 C43 P3 123.3(5) . . ? C37 C38 C39 121.1(6) . . ? C40 C39 C38 119.7(6) . . ? C29 C30 C25 121.9(6) . . ? C45 C44 C43 121.3(6) . . ? C25 C26 C27 121.2(6) . . ? C47 C48 C43 121.2(6) . . ? C46 C45 C44 119.4(7) . . ? C30 C29 C28 120.5(7) . . ? C28 C27 C26 120.6(7) . . ? C46 C47 C48 120.1(7) . . ? C47 C46 C45 120.7(7) . . ? C27 C28 C29 118.6(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.611 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.112 data_cuipph_mono_203k _database_code_depnum_ccdc_archive 'CCDC 777569' #TrackingRef 'mono-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method chloroform/ether _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 203(1) _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 0.0021 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 0.2614 1.2674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7268 1.8135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0905 0.0944 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 13.4801(3) _cell_length_b 26.6785(5) _cell_length_c 19.4749(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.1380(10) _cell_angle_gamma 90.00 _cell_volume 6914.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 3.132 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5861 _exptl_absorpt_correction_T_max 0.8166 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal focus sealed tube' _diffrn_source_type 'Rigaku R-AXIS' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID-F' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 120896 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 29.99 _reflns_number_total 19992 _reflns_number_gt 14635 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_cell_refinement 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2006), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0169P)^2^+6.4960P] 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 19992 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0657 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.003 _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 I4 I 0.485100(14) -0.199941(7) 0.343325(10) 0.03055(5) Uani 1 1 d . . . I3 I 0.176643(14) -0.193568(7) 0.216595(11) 0.03346(5) Uani 1 1 d . . . I2 I 0.435564(14) -0.138580(7) 0.130545(10) 0.03102(5) Uani 1 1 d . . . I1 I 0.325403(15) -0.062798(7) 0.311357(11) 0.03320(5) Uani 1 1 d . . . Cu1 Cu 0.37258(3) -0.206313(13) 0.21874(2) 0.03422(9) Uani 1 1 d . . . Cu4 Cu 0.29803(3) -0.162013(14) 0.33283(2) 0.03682(9) Uani 1 1 d . . . Cu2 Cu 0.47324(3) -0.115444(13) 0.26640(2) 0.03363(9) Uani 1 1 d . . . Cu3 Cu 0.27929(3) -0.110971(14) 0.19044(2) 0.03570(9) Uani 1 1 d . . . P1 P 0.40147(6) -0.28286(3) 0.17698(4) 0.02771(16) Uani 1 1 d . . . P4 P 0.24537(6) -0.17609(3) 0.43562(4) 0.03335(18) Uani 1 1 d . . . P2 P 0.61677(6) -0.07048(3) 0.28639(4) 0.02805(16) Uani 1 1 d . . . P3 P 0.17527(6) -0.06558(3) 0.11200(4) 0.03061(17) Uani 1 1 d . . . C10 C 0.2456(3) -0.41643(13) 0.2657(2) 0.0514(10) Uani 1 1 d . . . H10 H 0.2145 -0.4436 0.2846 0.062 Uiso 1 1 calc R . . C58 C 0.0806(3) -0.32595(14) 0.4552(2) 0.0634(11) Uani 1 1 d . . . H58 H 0.0450 -0.3559 0.4583 0.076 Uiso 1 1 calc R . . C9 C 0.2746(3) -0.42080(13) 0.2021(2) 0.0549(10) Uani 1 1 d . . . H9 H 0.2632 -0.4510 0.1772 0.066 Uiso 1 1 calc R . . C57 C 0.1300(3) -0.30354(14) 0.5142(2) 0.0561(10) Uani 1 1 d . . . H57 H 0.1280 -0.3182 0.5578 0.067 Uiso 1 1 calc R . . C11 C 0.2617(3) -0.37217(14) 0.3023(2) 0.0525(9) Uani 1 1 d . . . H11 H 0.2419 -0.3692 0.3463 0.063 Uiso 1 1 calc R . . C59 C 0.0832(4) -0.30458(15) 0.3916(2) 0.0726(14) Uani 1 1 d . . . H59 H 0.0489 -0.3197 0.3511 0.087 Uiso 1 1 calc R . . C8 C 0.3209(3) -0.38116(12) 0.17362(19) 0.0439(8) Uani 1 1 d . . . H8 H 0.3402 -0.3846 0.1296 0.053 Uiso 1 1 calc R . . C56 C 0.1828(3) -0.25938(13) 0.5100(2) 0.0470(9) Uani 1 1 d . . . H56 H 0.2167 -0.2444 0.5508 0.056 Uiso 1 1 calc R . . C12 C 0.3074(2) -0.33203(12) 0.27428(17) 0.0416(8) Uani 1 1 d . . . H12 H 0.3170 -0.3017 0.2991 0.050 Uiso 1 1 calc R . . C5 C 0.6724(3) -0.35768(16) 0.2177(3) 0.097(2) Uani 1 1 d . . . H5 H 0.6953 -0.3906 0.2270 0.117 Uiso 1 1 calc R . . C7 C 0.3388(2) -0.33616(11) 0.21008(16) 0.0321(7) Uani 1 1 d . . . C60 C 0.1365(3) -0.26041(13) 0.3870(2) 0.0564(10) Uani 1 1 d . . . H60 H 0.1388 -0.2462 0.3431 0.068 Uiso 1 1 calc R . . C6 C 0.5700(3) -0.34775(14) 0.2071(2) 0.0663(13) Uani 1 1 d . . . H6 H 0.5242 -0.3739 0.2102 0.080 Uiso 1 1 calc R . . C55 C 0.1861(2) -0.23710(11) 0.44610(18) 0.0380(7) Uani 1 1 d . . . C69 C 0.4874(3) -0.2101(2) 0.5830(3) 0.0737(13) Uani 1 1 d . . . H69 H 0.5273 -0.2385 0.5961 0.088 Uiso 1 1 calc R . . C68 C 0.4071(3) -0.21377(15) 0.5300(2) 0.0549(10) Uani 1 1 d . . . H68 H 0.3925 -0.2447 0.5075 0.066 Uiso 1 1 calc R . . C4 C 0.7403(3) -0.31973(16) 0.2149(3) 0.0765(15) Uani 1 1 d . . . H4 H 0.8096 -0.3266 0.2223 0.092 Uiso 1 1 calc R . . C70 C 0.5098(3) -0.1656(3) 0.6168(2) 0.0862(17) Uani 1 1 d . . . H70 H 0.5638 -0.1634 0.6537 0.103 Uiso 1 1 calc R . . C1 C 0.5349(2) -0.29959(11) 0.19188(16) 0.0330(7) Uani 1 1 d . . . C67 C 0.3474(2) -0.17255(12) 0.50949(17) 0.0387(7) Uani 1 1 d . . . C66 C 0.1208(4) -0.13297(15) 0.5236(3) 0.0767(15) Uani 1 1 d . . . H66 H 0.1525 -0.1545 0.5586 0.092 Uiso 1 1 calc R . . C13 C 0.3606(2) -0.28643(10) 0.08341(16) 0.0307(6) Uani 1 1 d . . . C18 C 0.2589(3) -0.28982(16) 0.05904(19) 0.0568(10) Uani 1 1 d . . . H18 H 0.2138 -0.2930 0.0910 0.068 Uiso 1 1 calc R . . C3 C 0.7069(3) -0.27226(14) 0.2015(2) 0.0553(10) Uani 1 1 d . . . H3 H 0.7533 -0.2462 0.1998 0.066 Uiso 1 1 calc R . . C71 C 0.4531(4) -0.1243(2) 0.5962(3) 0.0851(16) Uani 1 1 d . . . H71 H 0.4690 -0.0935 0.6187 0.102 Uiso 1 1 calc R . . C65 C 0.0442(4) -0.10142(17) 0.5367(3) 0.0952(19) Uani 1 1 d . . . H65 H 0.0239 -0.1018 0.5807 0.114 Uiso 1 1 calc R . . C17 C 0.2223(3) -0.28865(16) -0.0110(2) 0.0643(12) Uani 1 1 d . . . H17 H 0.1528 -0.2915 -0.0265 0.077 Uiso 1 1 calc R . . C14 C 0.4242(3) -0.28085(15) 0.03583(19) 0.0554(10) Uani 1 1 d . . . H14 H 0.4938 -0.2782 0.0511 0.066 Uiso 1 1 calc R . . C2 C 0.6050(2) -0.26188(11) 0.19017(18) 0.0405(8) Uani 1 1 d . . . H2 H 0.5830 -0.2287 0.1812 0.049 Uiso 1 1 calc R . . C72 C 0.3722(3) -0.12729(15) 0.5425(2) 0.0618(11) Uani 1 1 d . . . H72 H 0.3341 -0.0985 0.5286 0.074 Uiso 1 1 calc R . . C61 C 0.1505(2) -0.13266(11) 0.4584(2) 0.0410(8) Uani 1 1 d . . . C15 C 0.3870(4) -0.27907(19) -0.0347(2) 0.0770(14) Uani 1 1 d . . . H15 H 0.4315 -0.2748 -0.0669 0.092 Uiso 1 1 calc R . . C16 C 0.2861(4) -0.28348(15) -0.0581(2) 0.0620(11) Uani 1 1 d . . . H16 H 0.2613 -0.2829 -0.1060 0.074 Uiso 1 1 calc R . . C64 C -0.0024(3) -0.06952(15) 0.4861(3) 0.0738(14) Uani 1 1 d . . . H64 H -0.0548 -0.0486 0.4954 0.089 Uiso 1 1 calc R . . C62 C 0.1042(3) -0.10016(14) 0.4087(2) 0.0532(10) Uani 1 1 d . . . H62 H 0.1243 -0.0993 0.3647 0.064 Uiso 1 1 calc R . . C63 C 0.0273(3) -0.06834(16) 0.4230(3) 0.0679(13) Uani 1 1 d . . . H63 H -0.0037 -0.0462 0.3886 0.082 Uiso 1 1 calc R . . C33 C 0.8814(3) -0.14852(12) 0.2908(2) 0.0515(10) Uani 1 1 d . . . H33 H 0.9343 -0.1602 0.3244 0.062 Uiso 1 1 calc R . . C23 C 0.6491(4) -0.05824(19) 0.4976(2) 0.0920(18) Uani 1 1 d . . . H23 H 0.6223 -0.0742 0.5336 0.110 Uiso 1 1 calc R . . C52 C -0.0111(4) -0.16637(14) -0.0525(2) 0.0733(14) Uani 1 1 d . . . H52 H -0.0482 -0.1873 -0.0859 0.088 Uiso 1 1 calc R . . C34 C 0.8816(3) -0.15913(12) 0.2219(2) 0.0538(10) Uani 1 1 d . . . H34 H 0.9349 -0.1774 0.2083 0.065 Uiso 1 1 calc R . . C24 C 0.6189(3) -0.07315(16) 0.42895(19) 0.0637(12) Uani 1 1 d . . . H24 H 0.5712 -0.0989 0.4188 0.076 Uiso 1 1 calc R . . C51 C -0.0593(3) -0.13587(16) -0.0130(2) 0.0660(12) Uani 1 1 d . . . H51 H -0.1299 -0.1358 -0.0192 0.079 Uiso 1 1 calc R . . C53 C 0.0919(4) -0.16662(16) -0.0435(2) 0.0799(15) Uani 1 1 d . . . H53 H 0.1254 -0.1878 -0.0708 0.096 Uiso 1 1 calc R . . C32 C 0.8040(2) -0.12072(11) 0.31178(19) 0.0410(8) Uani 1 1 d . . . H32 H 0.8053 -0.1133 0.3591 0.049 Uiso 1 1 calc R . . C35 C 0.8032(3) -0.14286(12) 0.1725(2) 0.0462(8) Uani 1 1 d . . . H35 H 0.8031 -0.1498 0.1252 0.055 Uiso 1 1 calc R . . C54 C 0.1469(3) -0.13569(15) 0.0058(2) 0.0654(12) Uani 1 1 d . . . H54 H 0.2175 -0.1363 0.0119 0.078 Uiso 1 1 calc R . . C22 C 0.7177(4) -0.02047(16) 0.5127(2) 0.0708(13) Uani 1 1 d . . . H22 H 0.7379 -0.0105 0.5591 0.085 Uiso 1 1 calc R . . C31 C 0.7246(2) -0.10395(10) 0.26248(16) 0.0312(7) Uani 1 1 d . . . C50 C -0.0054(3) -0.10453(13) 0.03658(19) 0.0494(9) Uani 1 1 d . . . H50 H -0.0398 -0.0837 0.0637 0.059 Uiso 1 1 calc R . . C36 C 0.7248(2) -0.11629(11) 0.19298(17) 0.0374(7) Uani 1 1 d . . . H36 H 0.6706 -0.1063 0.1593 0.045 Uiso 1 1 calc R . . C49 C 0.0984(2) -0.10388(11) 0.04618(17) 0.0373(8) Uani 1 1 d . . . C19 C 0.6578(2) -0.05065(11) 0.37627(16) 0.0351(7) Uani 1 1 d . . . C42 C 0.0369(2) -0.05075(12) 0.19956(18) 0.0432(8) Uani 1 1 d . . . H42 H 0.0524 -0.0841 0.2124 0.052 Uiso 1 1 calc R . . C41 C -0.0332(3) -0.02489(14) 0.2307(2) 0.0499(9) Uani 1 1 d . . . H41 H -0.0668 -0.0410 0.2633 0.060 Uiso 1 1 calc R . . C21 C 0.7567(3) 0.00254(13) 0.4610(2) 0.0540(10) Uani 1 1 d . . . H21 H 0.8035 0.0286 0.4716 0.065 Uiso 1 1 calc R . . C20 C 0.7278(3) -0.01227(12) 0.39278(18) 0.0431(8) Uani 1 1 d . . . H20 H 0.7556 0.0037 0.3572 0.052 Uiso 1 1 calc R . . C37 C 0.0845(2) -0.02795(10) 0.14962(15) 0.0306(6) Uani 1 1 d . . . C40 C -0.0536(3) 0.02468(13) 0.2134(2) 0.0481(9) Uani 1 1 d . . . H40 H -0.1000 0.0426 0.2351 0.058 Uiso 1 1 calc R . . C25 C 0.6134(2) -0.01052(10) 0.23993(15) 0.0313(7) Uani 1 1 d . . . C43 C 0.2362(2) -0.02157(11) 0.06071(15) 0.0325(7) Uani 1 1 d . . . C38 C 0.0623(2) 0.02174(11) 0.13208(17) 0.0383(7) Uani 1 1 d . . . H38 H 0.0938 0.0377 0.0982 0.046 Uiso 1 1 calc R . . C39 C -0.0063(3) 0.04780(12) 0.16453(19) 0.0457(8) Uani 1 1 d . . . H39 H -0.0205 0.0815 0.1530 0.055 Uiso 1 1 calc R . . C30 C 0.5370(2) 0.02296(12) 0.24876(18) 0.0415(8) Uani 1 1 d . . . H30 H 0.4887 0.0137 0.2763 0.050 Uiso 1 1 calc R . . C44 C 0.3336(2) -0.00572(12) 0.08607(17) 0.0405(8) Uani 1 1 d . . . H44 H 0.3660 -0.0174 0.1294 0.049 Uiso 1 1 calc R . . C26 C 0.6813(2) 0.00402(12) 0.19801(18) 0.0410(8) Uani 1 1 d . . . H26 H 0.7335 -0.0179 0.1913 0.049 Uiso 1 1 calc R . . C48 C 0.1896(3) -0.00292(13) -0.00324(17) 0.0426(8) Uani 1 1 d . . . H48 H 0.1237 -0.0130 -0.0212 0.051 Uiso 1 1 calc R . . C45 C 0.3829(3) 0.02703(13) 0.0482(2) 0.0538(10) Uani 1 1 d . . . H45 H 0.4490 0.0371 0.0654 0.065 Uiso 1 1 calc R . . C29 C 0.5313(3) 0.06978(12) 0.2175(2) 0.0487(9) Uani 1 1 d . . . H29 H 0.4804 0.0923 0.2250 0.058 Uiso 1 1 calc R . . C27 C 0.6742(3) 0.05063(13) 0.16539(19) 0.0480(9) Uani 1 1 d . . . H27 H 0.7206 0.0596 0.1362 0.058 Uiso 1 1 calc R . . C47 C 0.2388(3) 0.03005(14) -0.04030(18) 0.0515(9) Uani 1 1 d . . . H47 H 0.2063 0.0424 -0.0832 0.062 Uiso 1 1 calc R . . C46 C 0.3352(3) 0.04506(14) -0.0150(2) 0.0571(10) Uani 1 1 d . . . H46 H 0.3687 0.0675 -0.0406 0.068 Uiso 1 1 calc R . . C28 C 0.5999(3) 0.08343(12) 0.17567(18) 0.0447(9) Uani 1 1 d . . . H28 H 0.5958 0.1151 0.1542 0.054 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 I4 0.02903(10) 0.03044(10) 0.02985(10) 0.00289(7) -0.00246(8) 0.00115(7) I3 0.02483(10) 0.03318(10) 0.04039(12) 0.00179(8) -0.00088(8) -0.00281(7) I2 0.03107(10) 0.03169(10) 0.02997(10) 0.00068(7) 0.00381(8) 0.00278(7) I1 0.03573(11) 0.02415(9) 0.04030(12) -0.00324(8) 0.00781(9) 0.00114(7) Cu1 0.0336(2) 0.02939(19) 0.0380(2) -0.00484(15) 0.00064(17) 0.00142(15) Cu4 0.0369(2) 0.0330(2) 0.0411(2) -0.00012(16) 0.00794(18) -0.00141(16) Cu2 0.0292(2) 0.03178(19) 0.0388(2) -0.00170(15) 0.00203(17) -0.00388(14) Cu3 0.0308(2) 0.0361(2) 0.0385(2) 0.00569(16) 0.00011(17) 0.00553(15) P1 0.0245(4) 0.0256(4) 0.0323(4) -0.0019(3) 0.0024(3) -0.0011(3) P4 0.0328(4) 0.0264(4) 0.0426(5) -0.0025(3) 0.0113(4) -0.0015(3) P2 0.0272(4) 0.0275(4) 0.0286(4) -0.0003(3) 0.0017(3) -0.0027(3) P3 0.0286(4) 0.0292(4) 0.0322(4) 0.0021(3) -0.0006(3) 0.0036(3) C10 0.042(2) 0.045(2) 0.066(3) 0.0172(18) 0.0059(19) -0.0100(16) C58 0.075(3) 0.038(2) 0.083(3) 0.004(2) 0.027(2) -0.0170(19) C9 0.058(2) 0.0377(19) 0.068(3) -0.0046(17) 0.007(2) -0.0174(17) C57 0.059(2) 0.048(2) 0.064(3) 0.0201(19) 0.015(2) -0.0061(18) C11 0.054(2) 0.060(2) 0.046(2) 0.0148(18) 0.0169(18) -0.0004(18) C59 0.104(4) 0.054(2) 0.064(3) -0.014(2) 0.027(3) -0.038(2) C8 0.048(2) 0.0353(17) 0.049(2) -0.0068(14) 0.0097(17) -0.0108(14) C56 0.043(2) 0.046(2) 0.053(2) 0.0088(16) 0.0094(17) -0.0018(15) C12 0.044(2) 0.0401(18) 0.041(2) 0.0030(14) 0.0068(16) -0.0023(14) C5 0.037(2) 0.050(3) 0.201(6) 0.056(3) 0.008(3) 0.0105(18) C7 0.0265(15) 0.0319(15) 0.0375(17) -0.0003(12) 0.0037(13) -0.0022(12) C60 0.081(3) 0.045(2) 0.049(2) -0.0100(16) 0.026(2) -0.0270(19) C6 0.034(2) 0.042(2) 0.121(4) 0.031(2) 0.004(2) -0.0009(15) C55 0.0408(18) 0.0279(15) 0.049(2) 0.0013(13) 0.0187(16) 0.0000(13) C69 0.041(2) 0.106(4) 0.074(3) 0.015(3) 0.006(2) 0.010(2) C68 0.038(2) 0.065(2) 0.062(3) 0.0007(19) 0.0079(19) 0.0047(17) C4 0.030(2) 0.063(3) 0.131(4) 0.042(3) -0.002(2) 0.0078(18) C70 0.046(3) 0.159(6) 0.051(3) -0.008(3) -0.002(2) -0.007(3) C1 0.0265(16) 0.0325(16) 0.0383(17) 0.0060(12) 0.0005(13) 0.0020(12) C67 0.0373(18) 0.0449(19) 0.0362(18) -0.0042(14) 0.0131(15) -0.0020(14) C66 0.098(4) 0.046(2) 0.104(4) 0.022(2) 0.071(3) 0.024(2) C13 0.0310(16) 0.0276(14) 0.0326(16) -0.0028(11) 0.0028(13) 0.0002(11) C18 0.033(2) 0.095(3) 0.040(2) -0.0007(19) -0.0008(17) 0.0024(19) C3 0.0341(19) 0.048(2) 0.082(3) 0.0166(19) 0.0012(19) -0.0077(15) C71 0.078(4) 0.108(4) 0.066(3) -0.041(3) 0.001(3) -0.021(3) C65 0.114(4) 0.057(3) 0.140(5) 0.016(3) 0.097(4) 0.021(3) C17 0.048(2) 0.089(3) 0.049(2) -0.004(2) -0.015(2) 0.010(2) C14 0.044(2) 0.081(3) 0.041(2) -0.0081(19) 0.0078(18) -0.0118(19) C2 0.0280(17) 0.0319(16) 0.060(2) 0.0057(14) 0.0027(15) -0.0025(12) C72 0.063(3) 0.060(2) 0.060(3) -0.019(2) 0.005(2) -0.006(2) C61 0.0321(17) 0.0277(16) 0.066(2) -0.0084(15) 0.0164(17) -0.0039(12) C15 0.080(3) 0.114(4) 0.039(2) -0.007(2) 0.017(2) -0.017(3) C16 0.082(3) 0.066(3) 0.033(2) -0.0056(18) -0.005(2) 0.000(2) C64 0.045(2) 0.046(2) 0.138(5) -0.018(3) 0.037(3) 0.0037(18) C62 0.036(2) 0.057(2) 0.062(3) -0.0188(18) -0.0073(18) 0.0091(16) C63 0.040(2) 0.066(3) 0.090(3) -0.024(2) -0.012(2) 0.0166(19) C33 0.0312(19) 0.0394(19) 0.079(3) 0.0068(18) -0.0058(19) 0.0056(14) C23 0.137(5) 0.105(4) 0.035(2) -0.012(2) 0.016(3) -0.051(3) C52 0.101(4) 0.039(2) 0.066(3) -0.0019(19) -0.030(3) -0.011(2) C34 0.036(2) 0.0348(18) 0.094(3) -0.0094(19) 0.018(2) -0.0025(14) C24 0.085(3) 0.071(3) 0.035(2) -0.0076(18) 0.009(2) -0.036(2) C51 0.063(3) 0.060(3) 0.066(3) 0.001(2) -0.016(2) -0.019(2) C53 0.106(4) 0.053(3) 0.069(3) -0.025(2) -0.021(3) 0.024(2) C32 0.0352(18) 0.0347(17) 0.050(2) 0.0064(14) -0.0043(16) 0.0001(13) C35 0.042(2) 0.0439(19) 0.056(2) -0.0080(16) 0.0161(18) -0.0050(15) C54 0.063(3) 0.060(2) 0.066(3) -0.024(2) -0.011(2) 0.021(2) C22 0.100(4) 0.066(3) 0.041(2) -0.023(2) -0.008(2) -0.008(2) C31 0.0280(16) 0.0259(14) 0.0401(18) 0.0022(12) 0.0064(13) -0.0042(11) C50 0.046(2) 0.044(2) 0.055(2) -0.0012(16) -0.0045(18) -0.0087(15) C36 0.0317(17) 0.0372(17) 0.0432(19) -0.0003(14) 0.0056(15) -0.0028(13) C49 0.0397(19) 0.0275(15) 0.0400(18) 0.0029(12) -0.0086(15) 0.0047(13) C19 0.0383(18) 0.0330(16) 0.0327(17) -0.0032(12) 0.0012(14) -0.0020(13) C42 0.0355(18) 0.0396(18) 0.056(2) 0.0119(15) 0.0105(16) 0.0045(14) C41 0.0361(19) 0.056(2) 0.061(2) 0.0105(18) 0.0188(18) 0.0054(16) C21 0.061(2) 0.0382(19) 0.053(2) -0.0110(16) -0.019(2) 0.0004(16) C20 0.046(2) 0.0370(17) 0.043(2) -0.0029(14) -0.0042(16) -0.0074(14) C37 0.0245(15) 0.0325(15) 0.0332(16) 0.0020(12) -0.0006(13) 0.0009(11) C40 0.0341(19) 0.049(2) 0.063(2) -0.0088(17) 0.0145(17) 0.0021(15) C25 0.0311(16) 0.0306(15) 0.0306(16) -0.0015(12) -0.0004(13) -0.0037(12) C43 0.0340(17) 0.0312(15) 0.0309(16) 0.0002(12) 0.0011(13) 0.0055(12) C38 0.0408(19) 0.0315(16) 0.0422(19) 0.0029(13) 0.0050(15) 0.0010(13) C39 0.048(2) 0.0326(17) 0.057(2) -0.0027(15) 0.0089(18) 0.0061(14) C30 0.0384(19) 0.0356(17) 0.052(2) 0.0044(14) 0.0121(16) 0.0000(14) C44 0.042(2) 0.0389(18) 0.0383(19) 0.0009(14) -0.0008(15) -0.0031(14) C26 0.0369(19) 0.0366(17) 0.051(2) 0.0076(14) 0.0120(16) 0.0029(13) C48 0.0374(19) 0.056(2) 0.0335(18) 0.0046(15) 0.0029(15) 0.0032(15) C45 0.053(2) 0.051(2) 0.054(2) 0.0045(17) 0.0000(19) -0.0184(17) C29 0.043(2) 0.0360(18) 0.066(3) 0.0041(16) 0.0041(18) 0.0062(15) C27 0.052(2) 0.0424(19) 0.052(2) 0.0133(16) 0.0164(18) -0.0014(16) C47 0.059(2) 0.064(2) 0.0316(19) 0.0101(16) 0.0089(18) 0.0021(19) C46 0.071(3) 0.055(2) 0.047(2) 0.0091(17) 0.015(2) -0.016(2) C28 0.048(2) 0.0313(17) 0.051(2) 0.0085(14) -0.0054(17) -0.0026(14) _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 I4 Cu1 2.6547(4) . ? I4 Cu4 2.6947(4) . ? I4 Cu2 2.6973(4) . ? I4 I1 4.2406(3) . ? I4 I2 4.4067(3) . ? I4 I3 4.4889(3) . ? I3 Cu1 2.6568(4) . ? I3 Cu3 2.6932(4) . ? I3 Cu4 2.7081(4) . ? I3 I1 4.2922(3) . ? I3 I2 4.3589(3) . ? I2 Cu3 2.6686(5) . ? I2 Cu2 2.6855(4) . ? I2 Cu1 2.7202(4) . ? I2 I1 4.5114(3) . ? I1 Cu3 2.6681(4) . ? I1 Cu2 2.6954(4) . ? I1 Cu4 2.7141(4) . ? Cu1 P1 2.2548(8) . ? Cu1 Cu4 2.8378(6) . ? Cu1 Cu3 2.8522(5) . ? Cu1 Cu2 2.8600(5) . ? Cu4 P4 2.2589(10) . ? Cu4 Cu3 3.0636(6) . ? Cu4 Cu2 3.1252(6) . ? Cu2 P2 2.2572(8) . ? Cu2 Cu3 2.7945(5) . ? Cu3 P3 2.2552(8) . ? P1 C13 1.820(3) . ? P1 C7 1.823(3) . ? P1 C1 1.831(3) . ? P4 C67 1.828(3) . ? P4 C61 1.832(3) . ? P4 C55 1.839(3) . ? P2 C31 1.828(3) . ? P2 C19 1.828(3) . ? P2 C25 1.835(3) . ? P3 C43 1.820(3) . ? P3 C37 1.824(3) . ? P3 C49 1.827(3) . ? C10 C9 1.362(5) . ? C10 C11 1.379(5) . ? C58 C59 1.368(6) . ? C58 C57 1.371(6) . ? C9 C8 1.387(5) . ? C57 C56 1.386(5) . ? C11 C12 1.389(5) . ? C59 C60 1.391(5) . ? C8 C7 1.396(4) . ? C56 C55 1.385(5) . ? C12 C7 1.387(4) . ? C5 C4 1.372(5) . ? C5 C6 1.388(5) . ? C60 C55 1.384(5) . ? C6 C1 1.385(4) . ? C69 C70 1.369(7) . ? C69 C68 1.376(6) . ? C68 C67 1.384(5) . ? C4 C3 1.356(5) . ? C70 C71 1.364(7) . ? C1 C2 1.384(4) . ? C67 C72 1.384(5) . ? C66 C65 1.387(6) . ? C66 C61 1.390(5) . ? C13 C14 1.366(5) . ? C13 C18 1.381(4) . ? C18 C17 1.376(5) . ? C3 C2 1.384(5) . ? C71 C72 1.389(6) . ? C65 C64 1.377(7) . ? C17 C16 1.360(6) . ? C14 C15 1.387(5) . ? C61 C62 1.374(5) . ? C15 C16 1.369(6) . ? C64 C63 1.353(6) . ? C62 C63 1.401(5) . ? C33 C34 1.373(5) . ? C33 C32 1.394(5) . ? C23 C22 1.368(6) . ? C23 C24 1.392(5) . ? C52 C51 1.354(6) . ? C52 C53 1.373(6) . ? C34 C35 1.381(5) . ? C24 C19 1.363(5) . ? C51 C50 1.392(5) . ? C53 C54 1.387(5) . ? C32 C31 1.393(4) . ? C35 C36 1.383(5) . ? C54 C49 1.389(5) . ? C22 C21 1.354(6) . ? C31 C36 1.393(4) . ? C50 C49 1.382(5) . ? C19 C20 1.395(4) . ? C42 C41 1.385(5) . ? C42 C37 1.388(4) . ? C41 C40 1.381(5) . ? C21 C20 1.382(5) . ? C37 C38 1.390(4) . ? C40 C39 1.373(5) . ? C25 C26 1.376(4) . ? C25 C30 1.394(4) . ? C43 C44 1.392(4) . ? C43 C48 1.395(4) . ? C38 C39 1.387(5) . ? C30 C29 1.386(4) . ? C44 C45 1.380(5) . ? C26 C27 1.393(4) . ? C48 C47 1.374(5) . ? C45 C46 1.381(5) . ? C29 C28 1.376(5) . ? C27 C28 1.368(5) . ? C47 C46 1.375(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I4 Cu4 64.072(13) . . ? Cu1 I4 Cu2 64.597(12) . . ? Cu4 I4 Cu2 70.843(12) . . ? Cu1 I4 I1 73.622(9) . . ? Cu4 I4 I1 38.533(9) . . ? Cu2 I4 I1 38.137(9) . . ? Cu1 I4 I2 35.420(9) . . ? Cu4 I4 I2 77.818(10) . . ? Cu2 I4 I2 34.962(9) . . ? I1 I4 I2 62.861(5) . . ? Cu1 I4 I3 32.329(9) . . ? Cu4 I4 I3 33.911(9) . . ? Cu2 I4 I3 72.238(9) . . ? I1 I4 I3 58.821(4) . . ? I2 I4 I3 58.675(4) . . ? Cu1 I3 Cu3 64.428(12) . . ? Cu1 I3 Cu4 63.862(13) . . ? Cu3 I3 Cu4 69.108(12) . . ? Cu1 I3 I1 72.654(9) . . ? Cu3 I3 I1 36.613(9) . . ? Cu4 I3 I1 37.714(9) . . ? Cu1 I3 I2 36.329(9) . . ? Cu3 I3 I2 35.426(9) . . ? Cu4 I3 I2 78.601(10) . . ? I1 I3 I2 62.858(5) . . ? Cu1 I3 I4 32.302(9) . . ? Cu3 I3 I4 71.102(9) . . ? Cu4 I3 I4 33.720(9) . . ? I1 I3 I4 57.701(4) . . ? I2 I3 I4 59.721(4) . . ? Cu3 I2 Cu2 62.924(12) . . ? Cu3 I2 Cu1 63.905(12) . . ? Cu2 I2 Cu1 63.882(12) . . ? Cu3 I2 I3 35.803(9) . . ? Cu2 I2 I3 74.709(10) . . ? Cu1 I2 I3 35.353(9) . . ? Cu3 I2 I4 72.767(9) . . ? Cu2 I2 I4 35.139(8) . . ? Cu1 I2 I4 34.446(8) . . ? I3 I2 I4 61.605(5) . . ? Cu3 I2 I1 32.285(9) . . ? Cu2 I2 I1 33.094(9) . . ? Cu1 I2 I1 68.311(9) . . ? I3 I2 I1 57.847(4) . . ? I4 I2 I1 56.770(4) . . ? Cu3 I1 Cu2 62.801(12) . . ? Cu3 I1 Cu4 69.385(12) . . ? Cu2 I1 Cu4 70.580(12) . . ? Cu3 I1 I4 75.857(9) . . ? Cu2 I1 I4 38.170(9) . . ? Cu4 I1 I4 38.207(9) . . ? Cu3 I1 I3 37.016(9) . . ? Cu2 I1 I3 75.867(9) . . ? Cu4 I1 I3 37.617(9) . . ? I4 I1 I3 63.477(5) . . ? Cu3 I1 I2 32.292(9) . . ? Cu2 I1 I2 32.957(9) . . ? Cu4 I1 I2 75.694(10) . . ? I4 I1 I2 60.369(4) . . ? I3 I1 I2 59.294(5) . . ? P1 Cu1 I4 106.34(2) . . ? P1 Cu1 I3 109.78(2) . . ? I4 Cu1 I3 115.369(16) . . ? P1 Cu1 I2 106.55(3) . . ? I4 Cu1 I2 110.134(14) . . ? I3 Cu1 I2 108.317(14) . . ? P1 Cu1 Cu4 139.69(3) . . ? I4 Cu1 Cu4 58.648(12) . . ? I3 Cu1 Cu4 58.949(12) . . ? I2 Cu1 Cu4 113.740(15) . . ? P1 Cu1 Cu3 146.53(3) . . ? I4 Cu1 Cu3 106.851(15) . . ? I3 Cu1 Cu3 58.406(11) . . ? I2 Cu1 Cu3 57.168(12) . . ? Cu4 Cu1 Cu3 65.152(14) . . ? P1 Cu1 Cu2 141.68(3) . . ? I4 Cu1 Cu2 58.423(11) . . ? I3 Cu1 Cu2 108.412(15) . . ? I2 Cu1 Cu2 57.469(11) . . ? Cu4 Cu1 Cu2 66.525(14) . . ? Cu3 Cu1 Cu2 58.579(13) . . ? P4 Cu4 I4 107.00(3) . . ? P4 Cu4 I3 117.12(3) . . ? I4 Cu4 I3 112.369(15) . . ? P4 Cu4 I1 111.61(2) . . ? I4 Cu4 I1 103.260(14) . . ? I3 Cu4 I1 104.669(14) . . ? P4 Cu4 Cu1 145.56(3) . . ? I4 Cu4 Cu1 57.280(12) . . ? I3 Cu4 Cu1 57.189(12) . . ? I1 Cu4 Cu1 102.226(16) . . ? P4 Cu4 Cu3 152.09(3) . . ? I4 Cu4 Cu3 100.205(15) . . ? I3 Cu4 Cu3 55.217(11) . . ? I1 Cu4 Cu3 54.599(11) . . ? Cu1 Cu4 Cu3 57.650(13) . . ? P4 Cu4 Cu2 142.88(3) . . ? I4 Cu4 Cu2 54.618(11) . . ? I3 Cu4 Cu2 99.994(15) . . ? I1 Cu4 Cu2 54.429(11) . . ? Cu1 Cu4 Cu2 57.077(13) . . ? Cu3 Cu4 Cu2 53.675(12) . . ? P2 Cu2 I2 108.35(3) . . ? P2 Cu2 I1 108.95(2) . . ? I2 Cu2 I1 113.948(14) . . ? P2 Cu2 I4 112.01(2) . . ? I2 Cu2 I4 109.899(14) . . ? I1 Cu2 I4 103.694(15) . . ? P2 Cu2 Cu3 140.61(3) . . ? I2 Cu2 Cu3 58.242(12) . . ? I1 Cu2 Cu3 58.122(12) . . ? I4 Cu2 Cu3 107.316(15) . . ? P2 Cu2 Cu1 148.87(3) . . ? I2 Cu2 Cu1 58.649(12) . . ? I1 Cu2 Cu1 102.121(15) . . ? I4 Cu2 Cu1 56.980(11) . . ? Cu3 Cu2 Cu1 60.570(13) . . ? P2 Cu2 Cu4 145.42(3) . . ? I2 Cu2 Cu4 106.224(14) . . ? I1 Cu2 Cu4 54.990(11) . . ? I4 Cu2 Cu4 54.539(11) . . ? Cu3 Cu2 Cu4 62.036(13) . . ? Cu1 Cu2 Cu4 56.398(13) . . ? P3 Cu3 I1 111.83(3) . . ? P3 Cu3 I2 107.53(3) . . ? I1 Cu3 I2 115.423(15) . . ? P3 Cu3 I3 106.53(2) . . ? I1 Cu3 I3 106.372(15) . . ? I2 Cu3 I3 108.771(14) . . ? P3 Cu3 Cu2 144.12(3) . . ? I1 Cu3 Cu2 59.077(12) . . ? I2 Cu3 Cu2 58.834(12) . . ? I3 Cu3 Cu2 109.300(15) . . ? P3 Cu3 Cu1 144.82(3) . . ? I1 Cu3 Cu1 103.018(14) . . ? I2 Cu3 Cu1 58.927(12) . . ? I3 Cu3 Cu1 57.166(11) . . ? Cu2 Cu3 Cu1 60.851(12) . . ? P3 Cu3 Cu4 143.59(3) . . ? I1 Cu3 Cu4 56.015(11) . . ? I2 Cu3 Cu4 108.400(14) . . ? I3 Cu3 Cu4 55.675(11) . . ? Cu2 Cu3 Cu4 64.289(13) . . ? Cu1 Cu3 Cu4 57.198(13) . . ? C13 P1 C7 103.29(13) . . ? C13 P1 C1 106.21(14) . . ? C7 P1 C1 104.63(13) . . ? C13 P1 Cu1 111.49(9) . . ? C7 P1 Cu1 117.55(10) . . ? C1 P1 Cu1 112.65(10) . . ? C67 P4 C61 104.07(15) . . ? C67 P4 C55 104.12(15) . . ? C61 P4 C55 101.58(14) . . ? C67 P4 Cu4 112.70(11) . . ? C61 P4 Cu4 116.08(12) . . ? C55 P4 Cu4 116.66(11) . . ? C31 P2 C19 104.69(14) . . ? C31 P2 C25 105.02(14) . . ? C19 P2 C25 101.54(13) . . ? C31 P2 Cu2 113.00(9) . . ? C19 P2 Cu2 116.06(11) . . ? C25 P2 Cu2 115.13(10) . . ? C43 P3 C37 104.80(13) . . ? C43 P3 C49 103.35(14) . . ? C37 P3 C49 104.37(14) . . ? C43 P3 Cu3 115.58(10) . . ? C37 P3 Cu3 114.08(10) . . ? C49 P3 Cu3 113.40(9) . . ? C9 C10 C11 120.0(3) . . ? C59 C58 C57 119.9(4) . . ? C10 C9 C8 120.7(3) . . ? C58 C57 C56 120.4(4) . . ? C10 C11 C12 120.0(4) . . ? C58 C59 C60 119.9(4) . . ? C9 C8 C7 120.3(3) . . ? C55 C56 C57 120.5(4) . . ? C7 C12 C11 120.7(3) . . ? C4 C5 C6 120.5(4) . . ? C12 C7 C8 118.3(3) . . ? C12 C7 P1 118.8(2) . . ? C8 C7 P1 122.9(3) . . ? C55 C60 C59 120.9(4) . . ? C1 C6 C5 120.4(3) . . ? C60 C55 C56 118.3(3) . . ? C60 C55 P4 117.8(3) . . ? C56 C55 P4 123.8(3) . . ? C70 C69 C68 120.6(4) . . ? C69 C68 C67 120.9(4) . . ? C3 C4 C5 119.6(4) . . ? C71 C70 C69 119.3(4) . . ? C2 C1 C6 117.9(3) . . ? C2 C1 P1 118.4(2) . . ? C6 C1 P1 123.6(2) . . ? C68 C67 C72 118.2(3) . . ? C68 C67 P4 121.1(3) . . ? C72 C67 P4 120.5(3) . . ? C65 C66 C61 119.7(4) . . ? C14 C13 C18 118.0(3) . . ? C14 C13 P1 123.4(2) . . ? C18 C13 P1 118.2(3) . . ? C17 C18 C13 121.3(4) . . ? C4 C3 C2 120.6(3) . . ? C70 C71 C72 120.7(4) . . ? C64 C65 C66 120.8(5) . . ? C16 C17 C18 120.4(4) . . ? C13 C14 C15 120.6(4) . . ? C1 C2 C3 121.0(3) . . ? C67 C72 C71 120.2(4) . . ? C62 C61 C66 118.8(3) . . ? C62 C61 P4 119.0(3) . . ? C66 C61 P4 122.1(3) . . ? C16 C15 C14 120.7(4) . . ? C17 C16 C15 119.1(4) . . ? C63 C64 C65 119.9(4) . . ? C61 C62 C63 120.7(4) . . ? C64 C63 C62 120.0(4) . . ? C34 C33 C32 120.9(3) . . ? C22 C23 C24 120.2(4) . . ? C51 C52 C53 119.8(4) . . ? C33 C34 C35 119.8(3) . . ? C19 C24 C23 120.5(4) . . ? C52 C51 C50 120.6(4) . . ? C52 C53 C54 120.3(4) . . ? C31 C32 C33 119.9(3) . . ? C34 C35 C36 119.7(4) . . ? C53 C54 C49 120.5(4) . . ? C21 C22 C23 120.1(4) . . ? C32 C31 C36 118.3(3) . . ? C32 C31 P2 122.4(3) . . ? C36 C31 P2 119.2(2) . . ? C49 C50 C51 120.5(4) . . ? C35 C36 C31 121.4(3) . . ? C50 C49 C54 118.2(3) . . ? C50 C49 P3 123.4(3) . . ? C54 C49 P3 118.3(3) . . ? C24 C19 C20 118.5(3) . . ? C24 C19 P2 119.9(2) . . ? C20 C19 P2 121.6(3) . . ? C41 C42 C37 120.8(3) . . ? C40 C41 C42 119.5(3) . . ? C22 C21 C20 120.1(3) . . ? C21 C20 C19 120.6(3) . . ? C42 C37 C38 119.0(3) . . ? C42 C37 P3 117.0(2) . . ? C38 C37 P3 123.9(3) . . ? C39 C40 C41 120.2(3) . . ? C26 C25 C30 117.8(3) . . ? C26 C25 P2 124.8(2) . . ? C30 C25 P2 117.3(2) . . ? C44 C43 C48 118.3(3) . . ? C44 C43 P3 118.9(2) . . ? C48 C43 P3 122.8(2) . . ? C39 C38 C37 120.0(3) . . ? C40 C39 C38 120.5(3) . . ? C29 C30 C25 120.9(3) . . ? C45 C44 C43 120.6(3) . . ? C25 C26 C27 121.2(3) . . ? C47 C48 C43 120.7(3) . . ? C44 C45 C46 120.1(3) . . ? C28 C29 C30 120.2(3) . . ? C28 C27 C26 120.2(3) . . ? C48 C47 C46 120.4(3) . . ? C47 C46 C45 119.8(3) . . ? C27 C28 C29 119.6(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.125 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.137 data_cuipph_mono_153k _database_code_depnum_ccdc_archive 'CCDC 777570' #TrackingRef 'mono-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method chloroform/ether _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 153(1) _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 0.0021 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 0.2614 1.2674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7268 1.8135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0905 0.0944 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 13.4525(3) _cell_length_b 26.5559(5) _cell_length_c 19.4660(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.2370(10) _cell_angle_gamma 90.00 _cell_volume 6863.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 3.155 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5841 _exptl_absorpt_correction_T_max 0.8155 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal focus sealed tube' _diffrn_source_type 'Rigaku R-AXIS' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID-F' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 119932 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 29.99 _reflns_number_total 19852 _reflns_number_gt 15920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_cell_refinement 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2006), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0155P)^2^+6.3631P] 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 19852 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0493 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 I4 I 0.487352(12) -0.200436(6) 0.342431(8) 0.02225(4) Uani 1 1 d . . . I3 I 0.178614(12) -0.194612(6) 0.214567(9) 0.02440(4) Uani 1 1 d . . . I2 I 0.438065(12) -0.138813(6) 0.129170(8) 0.02255(4) Uani 1 1 d . . . I1 I 0.327048(12) -0.062694(6) 0.309991(9) 0.02460(4) Uani 1 1 d . . . Cu1 Cu 0.37544(2) -0.206464(11) 0.217566(16) 0.02464(7) Uani 1 1 d . . . Cu4 Cu 0.29961(2) -0.162416(11) 0.330706(17) 0.02703(7) Uani 1 1 d . . . Cu2 Cu 0.47434(2) -0.115844(11) 0.265175(17) 0.02439(7) Uani 1 1 d . . . Cu3 Cu 0.28146(2) -0.111593(11) 0.189382(17) 0.02607(7) Uani 1 1 d . . . P1 P 0.40381(5) -0.28357(2) 0.17610(3) 0.02057(13) Uani 1 1 d . . . P4 P 0.24633(5) -0.17610(2) 0.43352(4) 0.02437(14) Uani 1 1 d . . . P2 P 0.61787(5) -0.07042(2) 0.28595(3) 0.02058(13) Uani 1 1 d . . . P3 P 0.17677(5) -0.06590(2) 0.11118(3) 0.02246(13) Uani 1 1 d . . . C10 C 0.2448(2) -0.41677(11) 0.26534(16) 0.0369(7) Uani 1 1 d . . . H10 H 0.2128 -0.4441 0.2845 0.044 Uiso 1 1 calc R . . C58 C 0.0812(2) -0.32666(11) 0.45400(18) 0.0454(8) Uani 1 1 d . . . H58 H 0.0447 -0.3569 0.4575 0.054 Uiso 1 1 calc R . . C9 C 0.2752(2) -0.42167(10) 0.20188(17) 0.0391(7) Uani 1 1 d . . . H9 H 0.2637 -0.4525 0.1770 0.047 Uiso 1 1 calc R . . C57 C 0.1331(2) -0.30463(11) 0.51286(18) 0.0424(7) Uani 1 1 d . . . H57 H 0.1327 -0.3199 0.5570 0.051 Uiso 1 1 calc R . . C11 C 0.2608(2) -0.37199(11) 0.30152(16) 0.0389(7) Uani 1 1 d . . . H11 H 0.2397 -0.3685 0.3456 0.047 Uiso 1 1 calc R . . C59 C 0.0820(3) -0.30493(11) 0.39014(18) 0.0500(9) Uani 1 1 d . . . H59 H 0.0464 -0.3202 0.3494 0.060 Uiso 1 1 calc R . . C8 C 0.3224(2) -0.38230(9) 0.17342(15) 0.0322(6) Uani 1 1 d . . . H8 H 0.3428 -0.3862 0.1292 0.039 Uiso 1 1 calc R . . C56 C 0.1862(2) -0.26023(10) 0.50835(16) 0.0342(6) Uani 1 1 d . . . H56 H 0.2221 -0.2454 0.5494 0.041 Uiso 1 1 calc R . . C12 C 0.3080(2) -0.33191(10) 0.27330(14) 0.0293(6) Uani 1 1 d . . . H12 H 0.3182 -0.3010 0.2981 0.035 Uiso 1 1 calc R . . C5 C 0.6749(2) -0.36002(12) 0.2129(2) 0.0674(13) Uani 1 1 d . . . H5 H 0.6979 -0.3936 0.2213 0.081 Uiso 1 1 calc R . . C7 C 0.34031(18) -0.33672(9) 0.20944(13) 0.0237(5) Uani 1 1 d . . . C60 C 0.1353(2) -0.26032(10) 0.38511(16) 0.0404(7) Uani 1 1 d . . . H60 H 0.1360 -0.2455 0.3408 0.048 Uiso 1 1 calc R . . C6 C 0.5719(2) -0.34971(11) 0.2034(2) 0.0482(9) Uani 1 1 d . . . H6 H 0.5252 -0.3762 0.2060 0.058 Uiso 1 1 calc R . . C55 C 0.1874(2) -0.23730(9) 0.44434(14) 0.0276(6) Uani 1 1 d . . . C69 C 0.4897(2) -0.20943(15) 0.5814(2) 0.0552(9) Uani 1 1 d . . . H69 H 0.5306 -0.2381 0.5948 0.066 Uiso 1 1 calc R . . C68 C 0.4099(2) -0.21323(12) 0.52756(17) 0.0400(7) Uani 1 1 d . . . H68 H 0.3970 -0.2443 0.5037 0.048 Uiso 1 1 calc R . . C4 C 0.7432(2) -0.32194(12) 0.2104(2) 0.0548(10) Uani 1 1 d . . . H4 H 0.8132 -0.3293 0.2169 0.066 Uiso 1 1 calc R . . C70 C 0.5107(3) -0.16450(18) 0.61594(19) 0.0636(11) Uani 1 1 d . . . H70 H 0.5654 -0.1621 0.6533 0.076 Uiso 1 1 calc R . . C1 C 0.53726(19) -0.30093(9) 0.19013(14) 0.0259(5) Uani 1 1 d . . . C67 C 0.3481(2) -0.17196(10) 0.50784(14) 0.0295(6) Uani 1 1 d . . . C66 C 0.1175(3) -0.13411(11) 0.5195(2) 0.0559(10) Uani 1 1 d . . . H66 H 0.1477 -0.1567 0.5546 0.067 Uiso 1 1 calc R . . C13 C 0.36166(19) -0.28702(9) 0.08255(13) 0.0235(5) Uani 1 1 d . . . C18 C 0.2594(2) -0.29254(12) 0.05843(16) 0.0412(7) Uani 1 1 d . . . H18 H 0.2144 -0.2976 0.0907 0.049 Uiso 1 1 calc R . . C3 C 0.7105(2) -0.27331(11) 0.19866(17) 0.0410(7) Uani 1 1 d . . . H3 H 0.7578 -0.2469 0.1972 0.049 Uiso 1 1 calc R . . C71 C 0.4520(3) -0.12331(16) 0.5960(2) 0.0632(11) Uani 1 1 d . . . H71 H 0.4669 -0.0921 0.6192 0.076 Uiso 1 1 calc R . . C65 C 0.0402(3) -0.10248(13) 0.5322(2) 0.0700(13) Uani 1 1 d . . . H65 H 0.0175 -0.1039 0.5760 0.084 Uiso 1 1 calc R . . C17 C 0.2221(2) -0.29073(13) -0.01207(17) 0.0477(8) Uani 1 1 d . . . H17 H 0.1520 -0.2949 -0.0278 0.057 Uiso 1 1 calc R . . C14 C 0.4245(2) -0.27875(12) 0.03471(16) 0.0413(7) Uani 1 1 d . . . H14 H 0.4947 -0.2743 0.0501 0.050 Uiso 1 1 calc R . . C2 C 0.60772(19) -0.26268(10) 0.18887(15) 0.0312(6) Uani 1 1 d . . . H2 H 0.5855 -0.2289 0.1812 0.037 Uiso 1 1 calc R . . C72 C 0.3708(2) -0.12666(12) 0.54197(17) 0.0452(8) Uani 1 1 d . . . H72 H 0.3308 -0.0978 0.5285 0.054 Uiso 1 1 calc R . . C61 C 0.1506(2) -0.13260(9) 0.45560(15) 0.0300(6) Uani 1 1 d . . . C15 C 0.3866(3) -0.27676(14) -0.03604(17) 0.0558(9) Uani 1 1 d . . . H15 H 0.4311 -0.2711 -0.0685 0.067 Uiso 1 1 calc R . . C16 C 0.2857(3) -0.28293(12) -0.05927(16) 0.0458(8) Uani 1 1 d . . . H16 H 0.2601 -0.2818 -0.1077 0.055 Uiso 1 1 calc R . . C64 C -0.0038(2) -0.06934(12) 0.4827(2) 0.0530(10) Uani 1 1 d . . . H64 H -0.0571 -0.0482 0.4918 0.064 Uiso 1 1 calc R . . C62 C 0.1061(2) -0.09875(11) 0.40583(16) 0.0381(7) Uani 1 1 d . . . H62 H 0.1280 -0.0973 0.3618 0.046 Uiso 1 1 calc R . . C63 C 0.0293(2) -0.06681(12) 0.41979(19) 0.0482(9) Uani 1 1 d . . . H63 H 0.0000 -0.0433 0.3856 0.058 Uiso 1 1 calc R . . C33 C 0.8833(2) -0.14919(10) 0.29291(18) 0.0393(7) Uani 1 1 d . . . H33 H 0.9363 -0.1611 0.3273 0.047 Uiso 1 1 calc R . . C23 C 0.6473(3) -0.05723(15) 0.49717(18) 0.0681(12) Uani 1 1 d . . . H23 H 0.6190 -0.0729 0.5334 0.082 Uiso 1 1 calc R . . C52 C -0.0113(3) -0.16686(11) -0.05387(17) 0.0530(10) Uani 1 1 d . . . H52 H -0.0489 -0.1881 -0.0878 0.064 Uiso 1 1 calc R . . C34 C 0.8844(2) -0.15988(10) 0.22409(18) 0.0409(8) Uani 1 1 d . . . H34 H 0.9387 -0.1785 0.2110 0.049 Uiso 1 1 calc R . . C24 C 0.6179(3) -0.07255(12) 0.42867(15) 0.0469(8) Uani 1 1 d . . . H24 H 0.5695 -0.0986 0.4184 0.056 Uiso 1 1 calc R . . C51 C -0.0598(3) -0.13563(12) -0.01464(18) 0.0481(8) Uani 1 1 d . . . H51 H -0.1313 -0.1351 -0.0213 0.058 Uiso 1 1 calc R . . C53 C 0.0924(3) -0.16754(13) -0.04403(19) 0.0616(11) Uani 1 1 d . . . H53 H 0.1264 -0.1893 -0.0713 0.074 Uiso 1 1 calc R . . C32 C 0.8051(2) -0.12096(9) 0.31282(16) 0.0316(6) Uani 1 1 d . . . H32 H 0.8055 -0.1133 0.3605 0.038 Uiso 1 1 calc R . . C35 C 0.8066(2) -0.14353(10) 0.17375(17) 0.0367(7) Uani 1 1 d . . . H35 H 0.8076 -0.1508 0.1261 0.044 Uiso 1 1 calc R . . C54 C 0.1475(3) -0.13664(12) 0.00530(17) 0.0484(9) Uani 1 1 d . . . H54 H 0.2190 -0.1375 0.0118 0.058 Uiso 1 1 calc R . . C22 C 0.7172(3) -0.01947(12) 0.51265(17) 0.0532(9) Uani 1 1 d . . . H22 H 0.7374 -0.0091 0.5595 0.064 Uiso 1 1 calc R . . C31 C 0.72633(18) -0.10398(8) 0.26276(13) 0.0235(5) Uani 1 1 d . . . C50 C -0.0051(2) -0.10440(11) 0.03532(15) 0.0371(7) Uani 1 1 d . . . H50 H -0.0396 -0.0830 0.0627 0.045 Uiso 1 1 calc R . . C36 C 0.7273(2) -0.11653(9) 0.19303(14) 0.0285(6) Uani 1 1 d . . . H36 H 0.6729 -0.1064 0.1585 0.034 Uiso 1 1 calc R . . C49 C 0.0990(2) -0.10436(9) 0.04535(14) 0.0288(6) Uani 1 1 d . . . C19 C 0.6584(2) -0.05024(9) 0.37547(13) 0.0262(5) Uani 1 1 d . . . C42 C 0.0373(2) -0.05164(10) 0.19837(15) 0.0319(6) Uani 1 1 d . . . H42 H 0.0527 -0.0856 0.2110 0.038 Uiso 1 1 calc R . . C41 C -0.0334(2) -0.02567(11) 0.22918(16) 0.0371(7) Uani 1 1 d . . . H41 H -0.0681 -0.0421 0.2616 0.044 Uiso 1 1 calc R . . C21 C 0.7578(2) 0.00318(10) 0.46052(16) 0.0405(8) Uani 1 1 d . . . H21 H 0.8058 0.0294 0.4713 0.049 Uiso 1 1 calc R . . C20 C 0.7291(2) -0.01187(10) 0.39202(15) 0.0322(6) Uani 1 1 d . . . H20 H 0.7577 0.0040 0.3561 0.039 Uiso 1 1 calc R . . C37 C 0.08589(18) -0.02820(9) 0.14885(13) 0.0231(5) Uani 1 1 d . . . C40 C -0.0533(2) 0.02440(11) 0.21241(16) 0.0353(6) Uani 1 1 d . . . H40 H -0.1008 0.0424 0.2340 0.042 Uiso 1 1 calc R . . C25 C 0.61406(19) -0.01019(9) 0.23928(13) 0.0240(5) Uani 1 1 d . . . C43 C 0.23777(19) -0.02167(9) 0.06001(13) 0.0242(5) Uani 1 1 d . . . C38 C 0.0645(2) 0.02186(9) 0.13207(14) 0.0278(6) Uani 1 1 d . . . H38 H 0.0970 0.0381 0.0983 0.033 Uiso 1 1 calc R . . C39 C -0.0043(2) 0.04828(10) 0.16441(15) 0.0345(6) Uani 1 1 d . . . H39 H -0.0176 0.0827 0.1535 0.041 Uiso 1 1 calc R . . C30 C 0.5378(2) 0.02342(9) 0.24820(15) 0.0305(6) Uani 1 1 d . . . H30 H 0.4892 0.0141 0.2763 0.037 Uiso 1 1 calc R . . C44 C 0.3355(2) -0.00589(9) 0.08531(14) 0.0293(6) Uani 1 1 d . . . H44 H 0.3686 -0.0179 0.1290 0.035 Uiso 1 1 calc R . . C26 C 0.6830(2) 0.00413(10) 0.19705(14) 0.0308(6) Uani 1 1 d . . . H26 H 0.7357 -0.0182 0.1903 0.037 Uiso 1 1 calc R . . C48 C 0.1898(2) -0.00273(10) -0.00400(14) 0.0315(6) Uani 1 1 d . . . H48 H 0.1231 -0.0131 -0.0220 0.038 Uiso 1 1 calc R . . C45 C 0.3848(2) 0.02721(11) 0.04730(16) 0.0399(7) Uani 1 1 d . . . H45 H 0.4519 0.0373 0.0646 0.048 Uiso 1 1 calc R . . C29 C 0.5318(2) 0.07053(10) 0.21638(16) 0.0360(7) Uani 1 1 d . . . H29 H 0.4800 0.0934 0.2236 0.043 Uiso 1 1 calc R . . C27 C 0.6756(2) 0.05100(10) 0.16442(16) 0.0373(7) Uani 1 1 d . . . H27 H 0.7227 0.0601 0.1351 0.045 Uiso 1 1 calc R . . C47 C 0.2390(2) 0.03093(11) -0.04115(15) 0.0378(7) Uani 1 1 d . . . H47 H 0.2056 0.0440 -0.0842 0.045 Uiso 1 1 calc R . . C46 C 0.3366(2) 0.04560(11) -0.01577(16) 0.0410(7) Uani 1 1 d . . . H46 H 0.3706 0.0683 -0.0417 0.049 Uiso 1 1 calc R . . C28 C 0.6008(2) 0.08413(10) 0.17442(15) 0.0337(6) Uani 1 1 d . . . H28 H 0.5966 0.1162 0.1525 0.040 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 I4 0.02123(8) 0.02205(8) 0.02168(8) 0.00210(6) -0.00194(6) 0.00099(6) I3 0.01793(8) 0.02417(8) 0.02968(9) 0.00148(6) -0.00055(7) -0.00215(6) I2 0.02258(8) 0.02292(8) 0.02191(8) 0.00058(6) 0.00288(6) 0.00204(6) I1 0.02651(9) 0.01739(7) 0.03038(9) -0.00278(6) 0.00599(7) 0.00103(6) Cu1 0.02412(16) 0.02081(15) 0.02775(17) -0.00330(11) 0.00045(13) 0.00105(11) Cu4 0.02723(17) 0.02378(15) 0.03048(17) -0.00078(12) 0.00584(14) -0.00103(12) Cu2 0.02117(16) 0.02283(15) 0.02832(17) -0.00131(12) 0.00138(13) -0.00293(11) Cu3 0.02198(16) 0.02609(16) 0.02880(17) 0.00425(12) -0.00001(13) 0.00402(12) P1 0.0181(3) 0.0193(3) 0.0237(3) -0.0009(2) 0.0014(3) -0.0009(2) P4 0.0237(3) 0.0192(3) 0.0317(4) -0.0027(2) 0.0086(3) -0.0009(2) P2 0.0206(3) 0.0195(3) 0.0209(3) -0.0003(2) 0.0011(3) -0.0021(2) P3 0.0212(3) 0.0212(3) 0.0237(3) 0.0012(2) 0.0000(3) 0.0025(2) C10 0.0298(15) 0.0323(15) 0.0487(19) 0.0096(13) 0.0068(14) -0.0075(11) C58 0.051(2) 0.0272(15) 0.061(2) 0.0029(14) 0.0179(17) -0.0112(13) C9 0.0389(17) 0.0258(14) 0.052(2) -0.0048(12) 0.0058(15) -0.0123(12) C57 0.0408(18) 0.0368(16) 0.051(2) 0.0162(14) 0.0117(15) -0.0024(13) C11 0.0363(17) 0.0446(17) 0.0378(17) 0.0094(13) 0.0115(14) 0.0011(13) C59 0.069(2) 0.0358(17) 0.049(2) -0.0117(14) 0.0195(18) -0.0228(15) C8 0.0348(15) 0.0258(13) 0.0371(16) -0.0049(11) 0.0090(13) -0.0066(11) C56 0.0327(15) 0.0318(15) 0.0386(16) 0.0047(11) 0.0071(13) 0.0004(11) C12 0.0279(14) 0.0299(14) 0.0299(14) 0.0005(10) 0.0037(12) -0.0012(10) C5 0.0301(18) 0.0341(18) 0.136(4) 0.035(2) 0.009(2) 0.0095(13) C7 0.0189(12) 0.0240(12) 0.0279(13) 0.0003(9) 0.0024(10) -0.0015(9) C60 0.057(2) 0.0310(15) 0.0368(17) -0.0053(12) 0.0187(15) -0.0163(13) C6 0.0268(16) 0.0300(15) 0.087(3) 0.0218(15) 0.0061(16) 0.0006(12) C55 0.0290(14) 0.0198(12) 0.0368(15) -0.0019(10) 0.0134(12) -0.0005(10) C69 0.0280(18) 0.079(3) 0.058(2) 0.0126(19) 0.0040(16) 0.0076(16) C68 0.0277(16) 0.0480(18) 0.0448(18) 0.0008(14) 0.0078(14) 0.0049(12) C4 0.0185(15) 0.0487(19) 0.095(3) 0.0277(18) 0.0014(17) 0.0064(13) C70 0.0318(19) 0.119(4) 0.038(2) -0.006(2) -0.0007(16) -0.006(2) C1 0.0221(13) 0.0249(12) 0.0299(14) 0.0038(10) 0.0015(11) 0.0018(9) C67 0.0247(14) 0.0365(15) 0.0292(14) -0.0033(11) 0.0106(11) -0.0023(11) C66 0.071(2) 0.0308(16) 0.079(3) 0.0161(16) 0.054(2) 0.0169(15) C13 0.0244(13) 0.0190(11) 0.0263(13) -0.0038(9) 0.0013(11) 0.0007(9) C18 0.0255(15) 0.067(2) 0.0302(16) 0.0003(14) 0.0012(13) 0.0009(13) C3 0.0244(15) 0.0364(16) 0.060(2) 0.0126(14) 0.0009(14) -0.0047(12) C71 0.054(2) 0.083(3) 0.050(2) -0.030(2) 0.0027(19) -0.018(2) C65 0.086(3) 0.042(2) 0.101(3) 0.009(2) 0.072(3) 0.0158(19) C17 0.0347(18) 0.065(2) 0.0382(18) -0.0060(15) -0.0108(15) 0.0038(15) C14 0.0350(17) 0.058(2) 0.0325(16) -0.0059(14) 0.0097(13) -0.0103(14) C2 0.0220(13) 0.0257(13) 0.0446(17) 0.0046(11) 0.0013(12) -0.0014(10) C72 0.0443(19) 0.0466(18) 0.0435(19) -0.0123(14) 0.0035(15) -0.0048(14) C61 0.0238(14) 0.0208(12) 0.0481(17) -0.0061(11) 0.0136(12) -0.0020(10) C15 0.060(2) 0.081(3) 0.0296(17) -0.0033(16) 0.0155(17) -0.0152(19) C16 0.062(2) 0.0463(18) 0.0260(16) -0.0026(13) -0.0019(16) 0.0018(15) C64 0.0332(18) 0.0322(17) 0.098(3) -0.0148(17) 0.0253(19) 0.0020(13) C62 0.0260(15) 0.0422(16) 0.0420(17) -0.0148(13) -0.0074(13) 0.0059(12) C63 0.0310(17) 0.0495(19) 0.059(2) -0.0137(16) -0.0094(16) 0.0123(14) C33 0.0227(14) 0.0253(14) 0.066(2) 0.0040(13) -0.0051(14) 0.0032(10) C23 0.105(3) 0.074(3) 0.0273(18) -0.0064(16) 0.016(2) -0.035(2) C52 0.076(3) 0.0268(16) 0.046(2) -0.0028(13) -0.0215(18) -0.0077(15) C34 0.0263(15) 0.0251(14) 0.073(2) -0.0068(14) 0.0133(15) -0.0010(11) C24 0.065(2) 0.0488(19) 0.0269(16) -0.0063(13) 0.0066(15) -0.0244(16) C51 0.0455(19) 0.0432(18) 0.049(2) 0.0018(15) -0.0112(16) -0.0146(14) C53 0.081(3) 0.0407(19) 0.055(2) -0.0199(16) -0.015(2) 0.0184(18) C32 0.0251(14) 0.0252(13) 0.0420(17) 0.0046(11) -0.0022(12) -0.0008(10) C35 0.0336(16) 0.0305(15) 0.0497(19) -0.0085(12) 0.0177(14) -0.0047(11) C54 0.0463(19) 0.0445(18) 0.049(2) -0.0159(15) -0.0082(16) 0.0151(14) C22 0.078(3) 0.0479(19) 0.0288(17) -0.0154(14) -0.0054(17) -0.0028(17) C31 0.0202(12) 0.0180(11) 0.0317(14) 0.0021(9) 0.0025(10) -0.0028(9) C50 0.0358(17) 0.0363(15) 0.0370(16) -0.0009(12) -0.0014(13) -0.0052(12) C36 0.0238(14) 0.0284(13) 0.0336(15) -0.0008(10) 0.0056(11) -0.0018(10) C49 0.0307(15) 0.0207(12) 0.0317(14) 0.0023(10) -0.0051(12) 0.0022(10) C19 0.0303(14) 0.0223(12) 0.0244(13) -0.0026(9) -0.0007(11) -0.0015(10) C42 0.0271(14) 0.0289(14) 0.0405(16) 0.0077(11) 0.0076(12) 0.0040(10) C41 0.0290(15) 0.0423(17) 0.0423(17) 0.0061(13) 0.0131(13) 0.0029(12) C21 0.0464(18) 0.0265(14) 0.0419(18) -0.0095(12) -0.0134(15) -0.0007(12) C20 0.0363(16) 0.0263(13) 0.0314(15) -0.0014(10) -0.0027(12) -0.0045(11) C37 0.0179(12) 0.0236(12) 0.0259(13) -0.0005(9) -0.0023(10) 0.0001(9) C40 0.0259(15) 0.0372(15) 0.0436(17) -0.0084(12) 0.0080(13) 0.0016(11) C25 0.0240(13) 0.0231(12) 0.0233(13) 0.0003(9) -0.0010(10) -0.0027(9) C43 0.0261(13) 0.0214(12) 0.0248(13) -0.0001(9) 0.0037(11) 0.0034(9) C38 0.0318(15) 0.0229(12) 0.0285(14) 0.0015(10) 0.0039(11) -0.0004(10) C39 0.0354(16) 0.0239(13) 0.0442(17) -0.0035(11) 0.0067(13) 0.0016(11) C30 0.0283(14) 0.0257(13) 0.0390(16) 0.0026(11) 0.0095(12) -0.0007(10) C44 0.0309(15) 0.0284(13) 0.0270(14) 0.0007(10) -0.0006(12) -0.0025(10) C26 0.0298(15) 0.0270(13) 0.0363(15) 0.0057(11) 0.0077(12) 0.0041(10) C48 0.0291(15) 0.0405(15) 0.0243(14) 0.0035(11) 0.0025(11) 0.0037(11) C45 0.0407(18) 0.0378(16) 0.0392(17) 0.0030(12) 0.0007(14) -0.0122(13) C29 0.0325(16) 0.0259(14) 0.0491(18) 0.0029(12) 0.0051(14) 0.0052(11) C27 0.0423(17) 0.0316(15) 0.0401(17) 0.0088(12) 0.0127(14) -0.0026(12) C47 0.0445(18) 0.0439(17) 0.0248(14) 0.0076(12) 0.0047(13) 0.0025(13) C46 0.052(2) 0.0388(16) 0.0340(16) 0.0045(12) 0.0123(15) -0.0112(14) C28 0.0370(16) 0.0241(13) 0.0373(16) 0.0062(11) -0.0020(13) -0.0005(11) _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 I4 Cu1 2.6505(3) . ? I4 Cu2 2.6933(3) . ? I4 Cu4 2.6954(4) . ? I4 I1 4.2417(2) . ? I4 I2 4.4122(2) . ? I4 I3 4.4889(2) . ? I3 Cu1 2.6577(4) . ? I3 Cu3 2.6894(4) . ? I3 Cu4 2.7037(4) . ? I3 I1 4.3034(2) . ? I3 I2 4.3593(2) . ? I2 Cu3 2.6697(4) . ? I2 Cu2 2.6841(4) . ? I2 Cu1 2.7136(4) . ? I2 I1 4.5159(2) . ? I1 Cu3 2.6669(4) . ? I1 Cu2 2.6896(4) . ? I1 Cu4 2.7129(3) . ? Cu1 P1 2.2559(7) . ? Cu1 Cu4 2.8250(5) . ? Cu1 Cu3 2.8327(4) . ? Cu1 Cu2 2.8327(4) . ? Cu4 P4 2.2610(8) . ? Cu4 Cu3 3.0387(5) . ? Cu4 Cu2 3.1055(5) . ? Cu2 P2 2.2575(7) . ? Cu2 Cu3 2.7736(4) . ? Cu3 P3 2.2549(7) . ? P1 C13 1.820(3) . ? P1 C7 1.822(2) . ? P1 C1 1.831(3) . ? P4 C67 1.828(3) . ? P4 C61 1.832(3) . ? P4 C55 1.835(3) . ? P2 C19 1.821(3) . ? P2 C31 1.827(3) . ? P2 C25 1.836(2) . ? P3 C43 1.819(3) . ? P3 C37 1.823(3) . ? P3 C49 1.830(3) . ? C10 C9 1.368(4) . ? C10 C11 1.381(4) . ? C58 C59 1.372(5) . ? C58 C57 1.373(4) . ? C9 C8 1.384(4) . ? C57 C56 1.389(4) . ? C11 C12 1.397(4) . ? C59 C60 1.396(4) . ? C8 C7 1.400(3) . ? C56 C55 1.389(4) . ? C12 C7 1.387(4) . ? C5 C4 1.373(4) . ? C5 C6 1.395(4) . ? C60 C55 1.391(4) . ? C6 C1 1.387(4) . ? C69 C70 1.376(5) . ? C69 C68 1.379(4) . ? C68 C67 1.392(4) . ? C4 C3 1.372(4) . ? C70 C71 1.368(6) . ? C1 C2 1.392(3) . ? C67 C72 1.384(4) . ? C66 C61 1.388(4) . ? C66 C65 1.390(4) . ? C13 C14 1.373(4) . ? C13 C18 1.388(4) . ? C18 C17 1.384(4) . ? C3 C2 1.394(4) . ? C71 C72 1.392(5) . ? C65 C64 1.368(5) . ? C17 C16 1.368(5) . ? C14 C15 1.391(4) . ? C61 C62 1.385(4) . ? C15 C16 1.371(5) . ? C64 C63 1.370(5) . ? C62 C63 1.396(4) . ? C33 C34 1.372(5) . ? C33 C32 1.397(4) . ? C23 C22 1.375(5) . ? C23 C24 1.390(4) . ? C52 C51 1.362(5) . ? C52 C53 1.379(5) . ? C34 C35 1.384(4) . ? C24 C19 1.379(4) . ? C51 C50 1.395(4) . ? C53 C54 1.384(4) . ? C32 C31 1.394(3) . ? C35 C36 1.386(4) . ? C54 C49 1.390(4) . ? C22 C21 1.366(5) . ? C31 C36 1.400(4) . ? C50 C49 1.382(4) . ? C19 C20 1.396(3) . ? C42 C41 1.387(4) . ? C42 C37 1.395(4) . ? C41 C40 1.385(4) . ? C21 C20 1.386(4) . ? C37 C38 1.388(3) . ? C40 C39 1.381(4) . ? C25 C26 1.387(4) . ? C25 C30 1.392(4) . ? C43 C44 1.392(4) . ? C43 C48 1.401(3) . ? C38 C39 1.389(4) . ? C30 C29 1.393(4) . ? C44 C45 1.385(4) . ? C26 C27 1.394(4) . ? C48 C47 1.383(4) . ? C45 C46 1.382(4) . ? C29 C28 1.379(4) . ? C27 C28 1.375(4) . ? C47 C46 1.383(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I4 Cu2 64.017(10) . . ? Cu1 I4 Cu4 63.793(10) . . ? Cu2 I4 Cu4 70.381(10) . . ? Cu1 I4 I1 73.453(7) . . ? Cu2 I4 I1 37.971(8) . . ? Cu4 I4 I1 38.490(7) . . ? Cu1 I4 I2 35.129(7) . . ? Cu2 I4 I2 34.797(7) . . ? Cu4 I4 I2 77.534(8) . . ? I1 I4 I2 62.875(4) . . ? Cu1 I4 I3 32.308(8) . . ? Cu2 I4 I3 71.954(7) . . ? Cu4 I4 I3 33.815(7) . . ? I1 I4 I3 58.983(4) . . ? I2 I4 I3 58.641(4) . . ? Cu1 I3 Cu3 63.975(10) . . ? Cu1 I3 Cu4 63.587(10) . . ? Cu3 I3 Cu4 68.587(10) . . ? Cu1 I3 I1 72.261(7) . . ? Cu3 I3 I1 36.362(8) . . ? Cu4 I3 I1 37.467(7) . . ? Cu1 I3 I2 36.180(7) . . ? Cu3 I3 I2 35.417(7) . . ? Cu4 I3 I2 78.461(8) . . ? I1 I3 I2 62.836(4) . . ? Cu1 I3 I4 32.210(7) . . ? Cu3 I3 I4 70.856(7) . . ? Cu4 I3 I4 33.697(7) . . ? I1 I3 I4 57.643(3) . . ? I2 I3 I4 59.801(4) . . ? Cu3 I2 Cu2 62.403(10) . . ? Cu3 I2 Cu1 63.491(10) . . ? Cu2 I2 Cu1 63.307(10) . . ? Cu3 I2 I3 35.717(7) . . ? Cu2 I2 I3 74.397(8) . . ? Cu1 I2 I3 35.322(7) . . ? Cu3 I2 I4 72.383(8) . . ? Cu2 I2 I4 34.934(7) . . ? Cu1 I2 I4 34.197(7) . . ? I3 I2 I4 61.558(4) . . ? Cu3 I2 I1 32.178(7) . . ? Cu2 I2 I1 32.859(7) . . ? Cu1 I2 I1 68.094(8) . . ? I3 I2 I1 57.977(4) . . ? I4 I2 I1 56.717(4) . . ? Cu3 I1 Cu2 62.368(10) . . ? Cu3 I1 Cu4 68.776(10) . . ? Cu2 I1 Cu4 70.174(10) . . ? Cu3 I1 I4 75.566(7) . . ? Cu2 I1 I4 38.033(7) . . ? Cu4 I1 I4 38.198(7) . . ? Cu3 I1 I3 36.719(8) . . ? Cu2 I1 I3 75.389(7) . . ? Cu4 I1 I3 37.319(7) . . ? I4 I1 I3 63.374(4) . . ? Cu3 I1 I2 32.217(7) . . ? Cu2 I1 I2 32.783(7) . . ? Cu4 I1 I2 75.452(8) . . ? I4 I1 I2 60.409(4) . . ? I3 I1 I2 59.187(4) . . ? P1 Cu1 I4 106.210(19) . . ? P1 Cu1 I3 108.95(2) . . ? I4 Cu1 I3 115.481(13) . . ? P1 Cu1 I2 106.64(2) . . ? I4 Cu1 I2 110.674(12) . . ? I3 Cu1 I2 108.499(11) . . ? P1 Cu1 Cu4 139.27(2) . . ? I4 Cu1 Cu4 58.876(10) . . ? I3 Cu1 Cu4 58.999(10) . . ? I2 Cu1 Cu4 114.075(12) . . ? P1 Cu1 Cu3 146.50(2) . . ? I4 Cu1 Cu3 107.100(12) . . ? I3 Cu1 Cu3 58.555(9) . . ? I2 Cu1 Cu3 57.500(10) . . ? Cu4 Cu1 Cu3 64.971(11) . . ? P1 Cu1 Cu2 142.24(2) . . ? I4 Cu1 Cu2 58.726(9) . . ? I3 Cu1 Cu2 108.693(12) . . ? I2 Cu1 Cu2 57.840(10) . . ? Cu4 Cu1 Cu2 66.583(11) . . ? Cu3 Cu1 Cu2 58.625(10) . . ? P4 Cu4 I4 106.90(2) . . ? P4 Cu4 I3 117.10(2) . . ? I4 Cu4 I3 112.489(12) . . ? P4 Cu4 I1 111.01(2) . . ? I4 Cu4 I1 103.312(12) . . ? I3 Cu4 I1 105.214(12) . . ? P4 Cu4 Cu1 146.00(2) . . ? I4 Cu4 Cu1 57.331(10) . . ? I3 Cu4 Cu1 57.414(10) . . ? I1 Cu4 Cu1 102.331(13) . . ? P4 Cu4 Cu3 151.88(2) . . ? I4 Cu4 Cu3 100.432(12) . . ? I3 Cu4 Cu3 55.483(9) . . ? I1 Cu4 Cu3 54.896(9) . . ? Cu1 Cu4 Cu3 57.637(11) . . ? P4 Cu4 Cu2 142.75(2) . . ? I4 Cu4 Cu2 54.779(9) . . ? I3 Cu4 Cu2 100.151(12) . . ? I1 Cu4 Cu2 54.562(9) . . ? Cu1 Cu4 Cu2 56.828(10) . . ? Cu3 Cu4 Cu2 53.657(10) . . ? P2 Cu2 I2 108.24(2) . . ? P2 Cu2 I1 108.36(2) . . ? I2 Cu2 I1 114.358(12) . . ? P2 Cu2 I4 111.626(19) . . ? I2 Cu2 I4 110.269(11) . . ? I1 Cu2 I4 103.995(12) . . ? P2 Cu2 Cu3 140.69(2) . . ? I2 Cu2 Cu3 58.544(10) . . ? I1 Cu2 Cu3 58.414(10) . . ? I4 Cu2 Cu3 107.601(12) . . ? P2 Cu2 Cu1 148.85(2) . . ? I2 Cu2 Cu1 58.854(10) . . ? I1 Cu2 Cu1 102.719(12) . . ? I4 Cu2 Cu1 57.258(9) . . ? Cu3 Cu2 Cu1 60.687(11) . . ? P2 Cu2 Cu4 145.21(2) . . ? I2 Cu2 Cu4 106.553(11) . . ? I1 Cu2 Cu4 55.264(9) . . ? I4 Cu2 Cu4 54.841(9) . . ? Cu3 Cu2 Cu4 61.940(11) . . ? Cu1 Cu2 Cu4 56.590(10) . . ? P3 Cu3 I1 111.27(2) . . ? P3 Cu3 I2 107.50(2) . . ? I1 Cu3 I2 115.605(12) . . ? P3 Cu3 I3 106.28(2) . . ? I1 Cu3 I3 106.919(12) . . ? I2 Cu3 I3 108.867(12) . . ? P3 Cu3 Cu2 144.15(2) . . ? I1 Cu3 Cu2 59.218(10) . . ? I2 Cu3 Cu2 59.053(10) . . ? I3 Cu3 Cu2 109.534(12) . . ? P3 Cu3 Cu1 145.11(2) . . ? I1 Cu3 Cu1 103.306(12) . . ? I2 Cu3 Cu1 59.009(10) . . ? I3 Cu3 Cu1 57.470(9) . . ? Cu2 Cu3 Cu1 60.689(10) . . ? P3 Cu3 Cu4 143.22(2) . . ? I1 Cu3 Cu4 56.328(9) . . ? I2 Cu3 Cu4 108.833(12) . . ? I3 Cu3 Cu4 55.930(9) . . ? Cu2 Cu3 Cu4 64.404(11) . . ? Cu1 Cu3 Cu4 57.392(11) . . ? C13 P1 C7 103.22(11) . . ? C13 P1 C1 106.09(12) . . ? C7 P1 C1 104.85(11) . . ? C13 P1 Cu1 111.11(8) . . ? C7 P1 Cu1 117.36(9) . . ? C1 P1 Cu1 113.16(8) . . ? C67 P4 C61 103.99(13) . . ? C67 P4 C55 104.18(12) . . ? C61 P4 C55 101.45(12) . . ? C67 P4 Cu4 112.78(9) . . ? C61 P4 Cu4 116.17(10) . . ? C55 P4 Cu4 116.62(9) . . ? C19 P2 C31 104.58(12) . . ? C19 P2 C25 101.39(11) . . ? C31 P2 C25 105.22(12) . . ? C19 P2 Cu2 116.41(9) . . ? C31 P2 Cu2 112.90(8) . . ? C25 P2 Cu2 114.94(8) . . ? C43 P3 C37 104.85(11) . . ? C43 P3 C49 103.55(12) . . ? C37 P3 C49 104.09(12) . . ? C43 P3 Cu3 115.43(8) . . ? C37 P3 Cu3 114.24(8) . . ? C49 P3 Cu3 113.41(8) . . ? C9 C10 C11 119.9(3) . . ? C59 C58 C57 120.0(3) . . ? C10 C9 C8 120.8(3) . . ? C58 C57 C56 120.5(3) . . ? C10 C11 C12 119.9(3) . . ? C58 C59 C60 120.0(3) . . ? C9 C8 C7 120.4(3) . . ? C57 C56 C55 120.6(3) . . ? C7 C12 C11 120.7(3) . . ? C4 C5 C6 120.5(3) . . ? C12 C7 C8 118.4(2) . . ? C12 C7 P1 118.69(19) . . ? C8 C7 P1 122.9(2) . . ? C55 C60 C59 120.7(3) . . ? C1 C6 C5 120.3(3) . . ? C56 C55 C60 118.3(2) . . ? C56 C55 P4 123.9(2) . . ? C60 C55 P4 117.6(2) . . ? C70 C69 C68 120.6(3) . . ? C69 C68 C67 120.7(3) . . ? C3 C4 C5 120.1(3) . . ? C71 C70 C69 119.4(3) . . ? C6 C1 C2 118.4(2) . . ? C6 C1 P1 123.7(2) . . ? C2 C1 P1 117.89(18) . . ? C72 C67 C68 118.4(3) . . ? C72 C67 P4 120.8(2) . . ? C68 C67 P4 120.6(2) . . ? C61 C66 C65 119.9(3) . . ? C14 C13 C18 118.2(3) . . ? C14 C13 P1 122.9(2) . . ? C18 C13 P1 118.4(2) . . ? C17 C18 C13 120.9(3) . . ? C4 C3 C2 119.9(3) . . ? C70 C71 C72 120.7(3) . . ? C64 C65 C66 121.0(4) . . ? C16 C17 C18 120.3(3) . . ? C13 C14 C15 120.7(3) . . ? C1 C2 C3 120.9(2) . . ? C67 C72 C71 120.3(3) . . ? C62 C61 C66 118.7(3) . . ? C62 C61 P4 119.1(2) . . ? C66 C61 P4 122.1(2) . . ? C16 C15 C14 120.6(3) . . ? C17 C16 C15 119.3(3) . . ? C65 C64 C63 119.7(3) . . ? C61 C62 C63 120.6(3) . . ? C64 C63 C62 120.1(3) . . ? C34 C33 C32 120.6(3) . . ? C22 C23 C24 120.2(3) . . ? C51 C52 C53 119.7(3) . . ? C33 C34 C35 120.1(3) . . ? C19 C24 C23 120.6(3) . . ? C52 C51 C50 120.4(3) . . ? C52 C53 C54 120.4(3) . . ? C31 C32 C33 120.1(3) . . ? C34 C35 C36 119.9(3) . . ? C53 C54 C49 120.5(3) . . ? C21 C22 C23 119.9(3) . . ? C32 C31 C36 118.4(2) . . ? C32 C31 P2 122.2(2) . . ? C36 C31 P2 119.22(19) . . ? C49 C50 C51 120.5(3) . . ? C35 C36 C31 120.9(3) . . ? C50 C49 C54 118.4(3) . . ? C50 C49 P3 123.5(2) . . ? C54 C49 P3 118.0(2) . . ? C24 C19 C20 118.5(2) . . ? C24 C19 P2 119.9(2) . . ? C20 C19 P2 121.6(2) . . ? C41 C42 C37 120.5(2) . . ? C40 C41 C42 119.7(3) . . ? C22 C21 C20 120.3(3) . . ? C21 C20 C19 120.5(3) . . ? C38 C37 C42 119.2(2) . . ? C38 C37 P3 124.0(2) . . ? C42 C37 P3 116.86(18) . . ? C39 C40 C41 120.4(3) . . ? C26 C25 C30 118.3(2) . . ? C26 C25 P2 124.31(19) . . ? C30 C25 P2 117.4(2) . . ? C44 C43 C48 118.7(2) . . ? C44 C43 P3 118.95(19) . . ? C48 C43 P3 122.3(2) . . ? C37 C38 C39 120.3(3) . . ? C40 C39 C38 120.0(3) . . ? C25 C30 C29 120.8(3) . . ? C45 C44 C43 120.5(2) . . ? C25 C26 C27 120.6(3) . . ? C47 C48 C43 120.4(3) . . ? C46 C45 C44 120.2(3) . . ? C28 C29 C30 120.1(3) . . ? C28 C27 C26 120.5(3) . . ? C46 C47 C48 120.1(3) . . ? C45 C46 C47 120.1(3) . . ? C27 C28 C29 119.6(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.081 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.132 data_cuipph_mono_103k _database_code_depnum_ccdc_archive 'CCDC 777571' #TrackingRef 'mono-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method chloroform/ether _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 103(1) _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 0.0021 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 0.2614 1.2674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7268 1.8135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0905 0.0944 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 13.4230(3) _cell_length_b 26.4422(5) _cell_length_c 19.4442(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.306(1) _cell_angle_gamma 90.00 _cell_volume 6810.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 103(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 3.180 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5819 _exptl_absorpt_correction_T_max 0.8142 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal focus sealed tube' _diffrn_source_type 'Rigaku R-AXIS' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID-F' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 110779 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 30.01 _reflns_number_total 19710 _reflns_number_gt 16449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_cell_refinement 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2006), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0159P)^2^+5.3716P] 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 19710 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0520 _refine_ls_wR_factor_gt 0.0473 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.002 _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 I4 I 0.489491(11) -0.200965(5) 0.341664(7) 0.01481(3) Uani 1 1 d . . . I3 I 0.180429(10) -0.195595(5) 0.212697(8) 0.01617(3) Uani 1 1 d . . . I2 I 0.440362(11) -0.139070(5) 0.127898(7) 0.01495(3) Uani 1 1 d . . . I1 I 0.328776(11) -0.062594(5) 0.308892(8) 0.01658(3) Uani 1 1 d . . . Cu1 Cu 0.37809(2) -0.206652(10) 0.216530(14) 0.01634(6) Uani 1 1 d . . . Cu4 Cu 0.30118(2) -0.162745(10) 0.328708(15) 0.01799(6) Uani 1 1 d . . . Cu2 Cu 0.47550(2) -0.116291(10) 0.264066(15) 0.01637(6) Uani 1 1 d . . . Cu3 Cu 0.28352(2) -0.112179(10) 0.188531(15) 0.01744(6) Uani 1 1 d . . . P1 P 0.40596(4) -0.28425(2) 0.17533(3) 0.01396(11) Uani 1 1 d . . . P4 P 0.24744(4) -0.17609(2) 0.43158(3) 0.01655(12) Uani 1 1 d . . . P2 P 0.61894(4) -0.07039(2) 0.28551(3) 0.01402(11) Uani 1 1 d . . . P3 P 0.17823(4) -0.06619(2) 0.11053(3) 0.01526(11) Uani 1 1 d . . . C10 C 0.24424(18) -0.41707(9) 0.26512(14) 0.0253(5) Uani 1 1 d . . . H10 H 0.2115 -0.4442 0.2844 0.030 Uiso 1 1 calc R . . C58 C 0.0821(2) -0.32733(9) 0.45263(15) 0.0294(6) Uani 1 1 d . . . H58 H 0.0459 -0.3578 0.4562 0.035 Uiso 1 1 calc R . . C9 C 0.27577(19) -0.42286(9) 0.20173(14) 0.0269(6) Uani 1 1 d . . . H9 H 0.2645 -0.4540 0.1773 0.032 Uiso 1 1 calc R . . C57 C 0.1363(2) -0.30554(9) 0.51185(14) 0.0285(6) Uani 1 1 d . . . H57 H 0.1369 -0.3211 0.5560 0.034 Uiso 1 1 calc R . . C11 C 0.26013(19) -0.37179(9) 0.30090(13) 0.0259(5) Uani 1 1 d . . . H11 H 0.2381 -0.3678 0.3446 0.031 Uiso 1 1 calc R . . C59 C 0.0806(2) -0.30486(9) 0.38845(15) 0.0325(6) Uani 1 1 d . . . H59 H 0.0430 -0.3197 0.3478 0.039 Uiso 1 1 calc R . . C8 C 0.32407(18) -0.38332(8) 0.17326(13) 0.0223(5) Uani 1 1 d . . . H8 H 0.3452 -0.3875 0.1293 0.027 Uiso 1 1 calc R . . C56 C 0.18981(18) -0.26091(9) 0.50700(13) 0.0233(5) Uani 1 1 d . . . H56 H 0.2273 -0.2463 0.5478 0.028 Uiso 1 1 calc R . . C12 C 0.30854(18) -0.33199(9) 0.27270(12) 0.0202(5) Uani 1 1 d . . . H12 H 0.3189 -0.3009 0.2973 0.024 Uiso 1 1 calc R . . C5 C 0.6769(2) -0.36205(10) 0.20920(18) 0.0418(8) Uani 1 1 d . . . H5 H 0.6997 -0.3959 0.2169 0.050 Uiso 1 1 calc R . . C7 C 0.34171(16) -0.33734(8) 0.20914(12) 0.0152(4) Uani 1 1 d . . . C60 C 0.1345(2) -0.26037(9) 0.38351(13) 0.0264(5) Uani 1 1 d . . . H60 H 0.1344 -0.2453 0.3391 0.032 Uiso 1 1 calc R . . C6 C 0.57392(19) -0.35143(9) 0.20081(15) 0.0298(6) Uani 1 1 d . . . H6 H 0.5270 -0.3779 0.2036 0.036 Uiso 1 1 calc R . . C55 C 0.18863(17) -0.23760(8) 0.44269(12) 0.0186(5) Uani 1 1 d . . . C69 C 0.4924(2) -0.20890(12) 0.58004(15) 0.0367(7) Uani 1 1 d . . . H69 H 0.5344 -0.2374 0.5930 0.044 Uiso 1 1 calc R . . C68 C 0.41206(19) -0.21281(10) 0.52550(14) 0.0276(6) Uani 1 1 d . . . H68 H 0.3999 -0.2439 0.5012 0.033 Uiso 1 1 calc R . . C4 C 0.74589(19) -0.32371(10) 0.20643(16) 0.0340(7) Uani 1 1 d . . . H4 H 0.8159 -0.3312 0.2118 0.041 Uiso 1 1 calc R . . C70 C 0.5117(2) -0.16374(13) 0.61555(15) 0.0411(7) Uani 1 1 d . . . H70 H 0.5661 -0.1612 0.6533 0.049 Uiso 1 1 calc R . . C1 C 0.53964(16) -0.30211(8) 0.18836(12) 0.0173(4) Uani 1 1 d . . . C67 C 0.34908(18) -0.17163(9) 0.50612(12) 0.0199(5) Uani 1 1 d . . . C66 C 0.1154(2) -0.13499(9) 0.51618(16) 0.0355(7) Uani 1 1 d . . . H66 H 0.1445 -0.1583 0.5508 0.043 Uiso 1 1 calc R . . C13 C 0.36276(17) -0.28781(8) 0.08179(12) 0.0165(4) Uani 1 1 d . . . C18 C 0.25998(19) -0.29501(10) 0.05795(13) 0.0280(6) Uani 1 1 d . . . H18 H 0.2156 -0.3015 0.0903 0.034 Uiso 1 1 calc R . . C3 C 0.71288(19) -0.27448(9) 0.19590(14) 0.0279(6) Uani 1 1 d . . . H3 H 0.7604 -0.2480 0.1946 0.033 Uiso 1 1 calc R . . C71 C 0.4509(2) -0.12232(12) 0.59560(16) 0.0424(8) Uani 1 1 d . . . H71 H 0.4647 -0.0910 0.6192 0.051 Uiso 1 1 calc R . . C65 C 0.0376(2) -0.10336(11) 0.52896(18) 0.0435(8) Uani 1 1 d . . . H65 H 0.0134 -0.1056 0.5721 0.052 Uiso 1 1 calc R . . C17 C 0.2222(2) -0.29274(10) -0.01271(14) 0.0322(6) Uani 1 1 d . . . H17 H 0.1523 -0.2983 -0.0284 0.039 Uiso 1 1 calc R . . C14 C 0.4250(2) -0.27712(10) 0.03369(13) 0.0276(6) Uani 1 1 d . . . H14 H 0.4949 -0.2714 0.0491 0.033 Uiso 1 1 calc R . . C2 C 0.61039(17) -0.26355(8) 0.18721(13) 0.0216(5) Uani 1 1 d . . . H2 H 0.5882 -0.2295 0.1804 0.026 Uiso 1 1 calc R . . C72 C 0.3701(2) -0.12598(10) 0.54139(14) 0.0301(6) Uani 1 1 d . . . H72 H 0.3289 -0.0972 0.5283 0.036 Uiso 1 1 calc R . . C61 C 0.15075(17) -0.13258(8) 0.45295(13) 0.0203(5) Uani 1 1 d . . . C15 C 0.3863(2) -0.27458(11) -0.03704(14) 0.0370(7) Uani 1 1 d . . . H15 H 0.4301 -0.2674 -0.0696 0.044 Uiso 1 1 calc R . . C16 C 0.2848(2) -0.28248(10) -0.06026(13) 0.0306(6) Uani 1 1 d . . . H16 H 0.2586 -0.2808 -0.1086 0.037 Uiso 1 1 calc R . . C64 C -0.0046(2) -0.06891(10) 0.47965(17) 0.0339(7) Uani 1 1 d . . . H64 H -0.0579 -0.0475 0.4887 0.041 Uiso 1 1 calc R . . C62 C 0.10792(18) -0.09754(9) 0.40343(13) 0.0244(5) Uani 1 1 d . . . H62 H 0.1313 -0.0953 0.3600 0.029 Uiso 1 1 calc R . . C63 C 0.0306(2) -0.06558(10) 0.41744(15) 0.0317(6) Uani 1 1 d . . . H63 H 0.0023 -0.0414 0.3837 0.038 Uiso 1 1 calc R . . C33 C 0.88495(19) -0.14976(9) 0.29499(15) 0.0284(6) Uani 1 1 d . . . H33 H 0.9372 -0.1619 0.3299 0.034 Uiso 1 1 calc R . . C23 C 0.6461(3) -0.05660(12) 0.49704(15) 0.0452(8) Uani 1 1 d . . . H23 H 0.6172 -0.0720 0.5333 0.054 Uiso 1 1 calc R . . C52 C -0.0115(2) -0.16721(9) -0.05505(14) 0.0345(7) Uani 1 1 d . . . H52 H -0.0493 -0.1883 -0.0892 0.041 Uiso 1 1 calc R . . C34 C 0.88737(18) -0.16064(9) 0.22598(15) 0.0289(6) Uani 1 1 d . . . H34 H 0.9420 -0.1794 0.2134 0.035 Uiso 1 1 calc R . . C24 C 0.6169(2) -0.07226(10) 0.42836(13) 0.0310(6) Uani 1 1 d . . . H24 H 0.5681 -0.0983 0.4179 0.037 Uiso 1 1 calc R . . C51 C -0.0602(2) -0.13542(10) -0.01577(14) 0.0321(6) Uani 1 1 d . . . H51 H -0.1319 -0.1348 -0.0226 0.039 Uiso 1 1 calc R . . C53 C 0.0930(2) -0.16846(10) -0.04484(15) 0.0409(8) Uani 1 1 d . . . H53 H 0.1268 -0.1905 -0.0720 0.049 Uiso 1 1 calc R . . C32 C 0.80679(18) -0.12125(8) 0.31393(14) 0.0229(5) Uani 1 1 d . . . H32 H 0.8067 -0.1134 0.3616 0.028 Uiso 1 1 calc R . . C35 C 0.80988(18) -0.14410(9) 0.17474(14) 0.0252(5) Uani 1 1 d . . . H35 H 0.8116 -0.1514 0.1271 0.030 Uiso 1 1 calc R . . C54 C 0.1484(2) -0.13756(10) 0.00490(14) 0.0324(6) Uani 1 1 d . . . H54 H 0.2201 -0.1389 0.0120 0.039 Uiso 1 1 calc R . . C22 C 0.7170(2) -0.01868(10) 0.51267(14) 0.0363(7) Uani 1 1 d . . . H22 H 0.7369 -0.0083 0.5597 0.044 Uiso 1 1 calc R . . C31 C 0.72828(17) -0.10401(8) 0.26326(12) 0.0168(4) Uani 1 1 d . . . C50 C -0.00513(19) -0.10398(9) 0.03428(13) 0.0242(5) Uani 1 1 d . . . H50 H -0.0394 -0.0821 0.0614 0.029 Uiso 1 1 calc R . . C36 C 0.72982(18) -0.11677(8) 0.19336(13) 0.0199(5) Uani 1 1 d . . . H36 H 0.6756 -0.1066 0.1584 0.024 Uiso 1 1 calc R . . C49 C 0.09988(18) -0.10470(8) 0.04451(12) 0.0194(5) Uani 1 1 d . . . C19 C 0.65876(17) -0.04989(8) 0.37524(12) 0.0182(5) Uani 1 1 d . . . C42 C 0.03751(18) -0.05232(9) 0.19738(12) 0.0213(5) Uani 1 1 d . . . H42 H 0.0524 -0.0866 0.2096 0.026 Uiso 1 1 calc R . . C41 C -0.03365(18) -0.02639(9) 0.22819(13) 0.0239(5) Uani 1 1 d . . . H41 H -0.0687 -0.0431 0.2603 0.029 Uiso 1 1 calc R . . C21 C 0.7588(2) 0.00401(9) 0.46060(13) 0.0264(6) Uani 1 1 d . . . H21 H 0.8071 0.0303 0.4715 0.032 Uiso 1 1 calc R . . C20 C 0.73048(18) -0.01136(8) 0.39187(13) 0.0215(5) Uani 1 1 d . . . H20 H 0.7598 0.0043 0.3560 0.026 Uiso 1 1 calc R . . C37 C 0.08740(16) -0.02846(8) 0.14855(11) 0.0154(4) Uani 1 1 d . . . C40 C -0.05327(18) 0.02426(9) 0.21168(13) 0.0231(5) Uani 1 1 d . . . H40 H -0.1013 0.0423 0.2331 0.028 Uiso 1 1 calc R . . C25 C 0.61540(17) -0.00987(8) 0.23870(11) 0.0158(4) Uani 1 1 d . . . C43 C 0.23894(17) -0.02154(8) 0.05931(11) 0.0162(4) Uani 1 1 d . . . C38 C 0.06627(18) 0.02216(8) 0.13228(12) 0.0190(5) Uani 1 1 d . . . H38 H 0.0996 0.0388 0.0991 0.023 Uiso 1 1 calc R . . C39 C -0.00332(18) 0.04849(9) 0.16434(13) 0.0236(5) Uani 1 1 d . . . H39 H -0.0165 0.0832 0.1537 0.028 Uiso 1 1 calc R . . C30 C 0.53849(18) 0.02391(8) 0.24770(13) 0.0206(5) Uani 1 1 d . . . H30 H 0.4900 0.0146 0.2760 0.025 Uiso 1 1 calc R . . C44 C 0.33745(18) -0.00614(8) 0.08441(12) 0.0200(5) Uani 1 1 d . . . H44 H 0.3709 -0.0186 0.1279 0.024 Uiso 1 1 calc R . . C26 C 0.68436(18) 0.00444(9) 0.19643(13) 0.0219(5) Uani 1 1 d . . . H26 H 0.7372 -0.0180 0.1898 0.026 Uiso 1 1 calc R . . C48 C 0.19025(18) -0.00229(9) -0.00453(12) 0.0214(5) Uani 1 1 d . . . H48 H 0.1233 -0.0126 -0.0224 0.026 Uiso 1 1 calc R . . C45 C 0.3870(2) 0.02726(9) 0.04651(13) 0.0267(5) Uani 1 1 d . . . H45 H 0.4544 0.0373 0.0637 0.032 Uiso 1 1 calc R . . C29 C 0.53222(19) 0.07104(9) 0.21569(13) 0.0244(5) Uani 1 1 d . . . H29 H 0.4801 0.0939 0.2227 0.029 Uiso 1 1 calc R . . C27 C 0.6770(2) 0.05142(9) 0.16356(13) 0.0252(5) Uani 1 1 d . . . H27 H 0.7241 0.0605 0.1341 0.030 Uiso 1 1 calc R . . C47 C 0.2394(2) 0.03171(9) -0.04158(13) 0.0262(5) Uani 1 1 d . . . H47 H 0.2055 0.0453 -0.0843 0.031 Uiso 1 1 calc R . . C46 C 0.3378(2) 0.04599(9) -0.01649(13) 0.0279(6) Uani 1 1 d . . . H46 H 0.3718 0.0687 -0.0426 0.033 Uiso 1 1 calc R . . C28 C 0.60165(19) 0.08486(8) 0.17371(13) 0.0233(5) Uani 1 1 d . . . H28 H 0.5975 0.1171 0.1520 0.028 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 I4 0.01405(7) 0.01454(6) 0.01462(7) 0.00131(5) -0.00131(5) 0.00070(5) I3 0.01192(7) 0.01578(7) 0.01986(7) 0.00093(5) -0.00026(6) -0.00138(5) I2 0.01491(7) 0.01504(7) 0.01474(7) 0.00041(5) 0.00194(5) 0.00133(5) I1 0.01788(7) 0.01144(6) 0.02078(7) -0.00200(5) 0.00416(6) 0.00070(5) Cu1 0.01616(14) 0.01374(13) 0.01832(14) -0.00207(10) 0.00038(11) 0.00052(10) Cu4 0.01815(14) 0.01556(13) 0.02047(14) -0.00105(10) 0.00371(12) -0.00046(10) Cu2 0.01440(14) 0.01461(13) 0.01942(14) -0.00104(10) 0.00070(11) -0.00187(10) Cu3 0.01465(14) 0.01700(13) 0.01975(14) 0.00265(10) 0.00000(11) 0.00240(10) P1 0.0126(3) 0.0127(2) 0.0161(3) -0.00058(19) 0.0010(2) -0.00051(19) P4 0.0156(3) 0.0130(3) 0.0219(3) -0.0023(2) 0.0054(2) -0.0010(2) P2 0.0142(3) 0.0131(3) 0.0142(3) -0.00019(19) 0.0008(2) -0.0013(2) P3 0.0146(3) 0.0141(3) 0.0163(3) 0.0009(2) 0.0004(2) 0.0014(2) C10 0.0196(13) 0.0220(12) 0.0337(14) 0.0076(10) 0.0024(11) -0.0045(9) C58 0.0306(15) 0.0165(12) 0.0437(16) 0.0018(10) 0.0134(12) -0.0061(10) C9 0.0250(14) 0.0215(12) 0.0339(15) -0.0030(10) 0.0039(11) -0.0088(10) C57 0.0267(14) 0.0258(13) 0.0337(15) 0.0099(10) 0.0074(12) 0.0004(10) C11 0.0268(14) 0.0286(13) 0.0236(13) 0.0062(10) 0.0083(11) 0.0023(10) C59 0.0405(17) 0.0247(13) 0.0342(15) -0.0081(11) 0.0122(13) -0.0137(11) C8 0.0241(13) 0.0183(11) 0.0251(13) -0.0032(9) 0.0060(10) -0.0021(9) C56 0.0219(13) 0.0211(12) 0.0271(13) 0.0024(9) 0.0045(10) 0.0005(9) C12 0.0207(12) 0.0193(11) 0.0205(12) 0.0002(8) 0.0026(10) 0.0004(9) C5 0.0222(14) 0.0231(13) 0.081(2) 0.0203(14) 0.0100(15) 0.0077(10) C7 0.0101(10) 0.0147(10) 0.0198(11) 0.0010(8) 0.0000(9) 0.0001(8) C60 0.0366(15) 0.0217(12) 0.0244(13) -0.0035(9) 0.0152(11) -0.0095(10) C6 0.0188(13) 0.0195(12) 0.0510(17) 0.0128(11) 0.0055(12) -0.0008(9) C55 0.0174(11) 0.0141(10) 0.0262(12) -0.0013(8) 0.0094(10) -0.0001(8) C69 0.0211(14) 0.0512(18) 0.0376(16) 0.0102(13) 0.0044(13) 0.0045(12) C68 0.0233(14) 0.0312(14) 0.0290(14) 0.0000(10) 0.0063(11) 0.0018(10) C4 0.0120(12) 0.0316(14) 0.0571(19) 0.0156(13) 0.0015(12) 0.0052(10) C70 0.0207(15) 0.077(2) 0.0254(15) -0.0048(14) 0.0016(12) -0.0062(14) C1 0.0117(11) 0.0194(11) 0.0206(11) 0.0023(8) 0.0021(9) 0.0005(8) C67 0.0173(12) 0.0246(12) 0.0193(12) -0.0026(9) 0.0073(10) -0.0029(9) C66 0.0435(17) 0.0213(13) 0.0499(18) 0.0092(11) 0.0324(14) 0.0094(11) C13 0.0169(11) 0.0137(10) 0.0183(11) -0.0024(8) 0.0012(9) 0.0012(8) C18 0.0200(13) 0.0405(15) 0.0229(13) 0.0010(10) 0.0017(11) -0.0003(10) C3 0.0170(12) 0.0248(13) 0.0414(16) 0.0076(11) 0.0035(11) -0.0043(9) C71 0.0369(18) 0.056(2) 0.0339(16) -0.0214(14) 0.0045(14) -0.0126(14) C65 0.0495(19) 0.0289(15) 0.062(2) 0.0055(13) 0.0397(17) 0.0096(13) C17 0.0226(14) 0.0441(16) 0.0266(14) -0.0039(11) -0.0060(12) 0.0031(11) C14 0.0245(14) 0.0371(14) 0.0223(13) -0.0040(10) 0.0069(11) -0.0080(11) C2 0.0146(11) 0.0173(11) 0.0318(13) 0.0027(9) 0.0004(10) -0.0004(8) C72 0.0296(15) 0.0285(13) 0.0320(15) -0.0095(11) 0.0045(12) -0.0037(11) C61 0.0162(11) 0.0130(10) 0.0331(13) -0.0058(9) 0.0077(10) -0.0008(8) C15 0.0430(18) 0.0496(18) 0.0197(13) -0.0021(12) 0.0086(13) -0.0102(13) C16 0.0435(17) 0.0296(14) 0.0169(12) -0.0024(10) -0.0010(12) 0.0013(11) C64 0.0188(13) 0.0240(13) 0.061(2) -0.0112(12) 0.0138(13) 0.0021(10) C62 0.0178(12) 0.0279(13) 0.0256(13) -0.0081(10) -0.0027(10) 0.0022(9) C63 0.0212(13) 0.0319(14) 0.0380(16) -0.0105(11) -0.0076(12) 0.0084(10) C33 0.0167(12) 0.0181(12) 0.0478(17) 0.0033(11) -0.0027(12) 0.0013(9) C23 0.071(2) 0.0464(18) 0.0196(14) -0.0038(12) 0.0109(15) -0.0210(16) C52 0.0488(18) 0.0174(12) 0.0308(14) -0.0011(10) -0.0130(13) -0.0040(11) C34 0.0171(12) 0.0163(12) 0.0548(18) -0.0043(11) 0.0105(12) -0.0012(9) C24 0.0429(17) 0.0298(14) 0.0203(13) -0.0037(10) 0.0052(12) -0.0151(11) C51 0.0297(15) 0.0302(14) 0.0322(15) 0.0024(11) -0.0076(12) -0.0086(11) C53 0.053(2) 0.0261(14) 0.0377(16) -0.0114(11) -0.0097(15) 0.0141(13) C32 0.0190(12) 0.0179(11) 0.0297(13) 0.0028(9) -0.0024(11) -0.0010(9) C35 0.0230(13) 0.0204(12) 0.0349(14) -0.0053(10) 0.0129(11) -0.0045(9) C54 0.0295(15) 0.0309(14) 0.0326(15) -0.0109(11) -0.0075(12) 0.0099(11) C22 0.0532(19) 0.0336(15) 0.0185(13) -0.0095(10) -0.0050(13) -0.0004(13) C31 0.0144(11) 0.0116(10) 0.0246(12) 0.0006(8) 0.0037(9) -0.0023(8) C50 0.0228(13) 0.0221(12) 0.0262(13) 0.0004(9) -0.0011(11) -0.0032(9) C36 0.0167(12) 0.0178(11) 0.0255(13) -0.0015(9) 0.0043(10) -0.0020(8) C49 0.0222(12) 0.0143(10) 0.0193(11) 0.0017(8) -0.0041(10) 0.0018(8) C19 0.0194(12) 0.0157(10) 0.0184(11) -0.0011(8) -0.0006(9) 0.0001(8) C42 0.0195(12) 0.0189(11) 0.0250(12) 0.0046(9) 0.0026(10) 0.0013(9) C41 0.0178(12) 0.0300(13) 0.0253(13) 0.0039(10) 0.0072(10) 0.0000(9) C21 0.0291(14) 0.0178(11) 0.0276(13) -0.0055(9) -0.0098(11) -0.0001(9) C20 0.0211(12) 0.0190(11) 0.0223(12) -0.0009(9) -0.0034(10) -0.0025(9) C37 0.0113(10) 0.0171(10) 0.0162(11) -0.0014(8) -0.0030(9) 0.0004(8) C40 0.0164(12) 0.0264(12) 0.0268(13) -0.0067(9) 0.0041(10) 0.0012(9) C25 0.0170(11) 0.0150(10) 0.0144(10) -0.0009(8) -0.0001(9) -0.0016(8) C43 0.0157(11) 0.0162(10) 0.0171(11) -0.0007(8) 0.0038(9) 0.0011(8) C38 0.0209(12) 0.0172(11) 0.0191(11) 0.0014(8) 0.0042(10) -0.0004(8) C39 0.0230(13) 0.0185(11) 0.0296(13) -0.0012(9) 0.0048(11) 0.0022(9) C30 0.0171(12) 0.0183(11) 0.0271(13) 0.0024(9) 0.0055(10) -0.0017(8) C44 0.0212(12) 0.0186(11) 0.0186(11) 0.0009(8) -0.0016(10) -0.0008(9) C26 0.0209(12) 0.0198(11) 0.0255(12) 0.0032(9) 0.0053(10) 0.0016(9) C48 0.0197(12) 0.0268(12) 0.0176(11) 0.0008(9) 0.0023(10) 0.0015(9) C45 0.0258(14) 0.0266(13) 0.0270(13) 0.0013(10) 0.0015(11) -0.0076(10) C29 0.0214(13) 0.0171(11) 0.0342(14) 0.0012(9) 0.0028(11) 0.0047(9) C27 0.0277(14) 0.0223(12) 0.0269(13) 0.0041(9) 0.0080(11) -0.0011(10) C47 0.0303(14) 0.0315(13) 0.0171(12) 0.0050(9) 0.0045(11) 0.0039(10) C46 0.0363(15) 0.0247(13) 0.0241(13) 0.0036(10) 0.0091(12) -0.0071(10) C28 0.0259(13) 0.0163(11) 0.0252(13) 0.0040(9) -0.0032(11) -0.0006(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I4 Cu1 2.6461(3) . ? I4 Cu2 2.6895(3) . ? I4 Cu4 2.6960(3) . ? I4 I1 4.2429(2) . ? I4 I2 4.4163(2) . ? I4 I3 4.4894(2) . ? I3 Cu1 2.6583(3) . ? I3 Cu3 2.6854(3) . ? I3 Cu4 2.6995(3) . ? I3 I1 4.3159(2) . ? I3 I2 4.3574(2) . ? I2 Cu3 2.6703(3) . ? I2 Cu2 2.6817(3) . ? I2 Cu1 2.7070(3) . ? I2 I1 4.5192(2) . ? I1 Cu3 2.6656(3) . ? I1 Cu2 2.6851(3) . ? I1 Cu4 2.7101(3) . ? Cu1 P1 2.2559(6) . ? Cu1 Cu2 2.8075(4) . ? Cu1 Cu4 2.8106(4) . ? Cu1 Cu3 2.8151(4) . ? Cu4 P4 2.2610(7) . ? Cu4 Cu3 3.0107(4) . ? Cu4 Cu2 3.0846(4) . ? Cu2 P2 2.2571(6) . ? Cu2 Cu3 2.7541(4) . ? Cu3 P3 2.2546(6) . ? P1 C13 1.820(2) . ? P1 C7 1.825(2) . ? P1 C1 1.833(2) . ? P4 C67 1.827(2) . ? P4 C61 1.832(2) . ? P4 C55 1.836(2) . ? P2 C19 1.823(2) . ? P2 C31 1.827(2) . ? P2 C25 1.838(2) . ? P3 C43 1.820(2) . ? P3 C37 1.822(2) . ? P3 C49 1.831(2) . ? C10 C9 1.375(4) . ? C10 C11 1.384(4) . ? C58 C59 1.379(4) . ? C58 C57 1.384(4) . ? C9 C8 1.391(3) . ? C57 C56 1.393(3) . ? C11 C12 1.395(3) . ? C59 C60 1.393(3) . ? C8 C7 1.403(3) . ? C56 C55 1.392(3) . ? C12 C7 1.387(3) . ? C5 C4 1.380(4) . ? C5 C6 1.394(4) . ? C60 C55 1.394(3) . ? C6 C1 1.391(3) . ? C69 C70 1.383(4) . ? C69 C68 1.389(4) . ? C68 C67 1.393(3) . ? C4 C3 1.380(4) . ? C70 C71 1.383(5) . ? C1 C2 1.396(3) . ? C67 C72 1.394(3) . ? C66 C61 1.389(4) . ? C66 C65 1.391(4) . ? C13 C14 1.380(3) . ? C13 C18 1.396(3) . ? C18 C17 1.387(4) . ? C3 C2 1.389(3) . ? C71 C72 1.388(4) . ? C65 C64 1.376(4) . ? C17 C16 1.374(4) . ? C14 C15 1.391(4) . ? C61 C62 1.392(3) . ? C15 C16 1.380(4) . ? C64 C63 1.371(4) . ? C62 C63 1.399(3) . ? C33 C34 1.378(4) . ? C33 C32 1.389(3) . ? C23 C22 1.382(4) . ? C23 C24 1.393(4) . ? C52 C51 1.371(4) . ? C52 C53 1.384(4) . ? C34 C35 1.389(4) . ? C24 C19 1.386(3) . ? C51 C50 1.397(3) . ? C53 C54 1.387(4) . ? C32 C31 1.398(3) . ? C35 C36 1.391(3) . ? C54 C49 1.391(3) . ? C22 C21 1.372(4) . ? C31 C36 1.404(3) . ? C50 C49 1.391(3) . ? C19 C20 1.403(3) . ? C42 C41 1.388(3) . ? C42 C37 1.398(3) . ? C41 C40 1.392(3) . ? C21 C20 1.390(3) . ? C37 C38 1.394(3) . ? C40 C39 1.381(3) . ? C25 C26 1.386(3) . ? C25 C30 1.397(3) . ? C43 C44 1.394(3) . ? C43 C48 1.402(3) . ? C38 C39 1.391(3) . ? C30 C29 1.390(3) . ? C44 C45 1.387(3) . ? C26 C27 1.393(3) . ? C48 C47 1.384(3) . ? C45 C46 1.386(3) . ? C29 C28 1.384(4) . ? C27 C28 1.382(3) . ? C47 C46 1.386(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I4 Cu2 63.489(8) . . ? Cu1 I4 Cu4 63.481(9) . . ? Cu2 I4 Cu4 69.887(9) . . ? Cu1 I4 I1 73.316(7) . . ? Cu2 I4 I1 37.829(7) . . ? Cu4 I4 I1 38.413(6) . . ? Cu1 I4 I2 34.862(6) . . ? Cu2 I4 I2 34.635(6) . . ? Cu4 I4 I2 77.178(7) . . ? I1 I4 I2 62.881(3) . . ? Cu1 I4 I3 32.267(7) . . ? Cu2 I4 I3 71.693(7) . . ? Cu4 I4 I3 33.715(6) . . ? I1 I4 I3 59.160(3) . . ? I2 I4 I3 58.580(3) . . ? Cu1 I3 Cu3 63.577(9) . . ? Cu1 I3 Cu4 63.275(9) . . ? Cu3 I3 Cu4 67.986(9) . . ? Cu1 I3 I1 71.882(7) . . ? Cu3 I3 I1 36.083(7) . . ? Cu4 I3 I1 37.163(6) . . ? Cu1 I3 I2 36.070(6) . . ? Cu3 I3 I2 35.435(7) . . ? Cu4 I3 I2 78.260(7) . . ? I1 I3 I2 62.802(3) . . ? Cu1 I3 I4 32.102(7) . . ? Cu3 I3 I4 70.605(7) . . ? Cu4 I3 I4 33.664(6) . . ? I1 I3 I4 57.574(3) . . ? I2 I3 I4 59.872(3) . . ? Cu3 I2 Cu2 61.940(9) . . ? Cu3 I2 Cu1 63.131(9) . . ? Cu2 I2 Cu1 62.796(8) . . ? Cu3 I2 I3 35.665(6) . . ? Cu2 I2 I3 74.168(7) . . ? Cu1 I2 I3 35.322(6) . . ? Cu3 I2 I4 72.033(7) . . ? Cu2 I2 I4 34.750(6) . . ? Cu1 I2 I4 33.969(6) . . ? I3 I2 I4 61.548(3) . . ? Cu3 I2 I1 32.088(6) . . ? Cu2 I2 I1 32.664(6) . . ? Cu1 I2 I1 67.931(7) . . ? I3 I2 I1 58.150(3) . . ? I4 I2 I1 56.684(3) . . ? Cu3 I1 Cu2 61.957(9) . . ? Cu3 I1 Cu4 68.112(9) . . ? Cu2 I1 Cu4 69.741(9) . . ? Cu3 I1 I4 75.276(7) . . ? Cu2 I1 I4 37.902(6) . . ? Cu4 I1 I4 38.176(7) . . ? Cu3 I1 I3 36.393(7) . . ? Cu2 I1 I3 74.909(7) . . ? Cu4 I1 I3 36.993(6) . . ? I4 I1 I3 63.266(3) . . ? Cu3 I1 I2 32.151(7) . . ? Cu2 I1 I2 32.618(6) . . ? Cu4 I1 I2 75.144(7) . . ? I4 I1 I2 60.435(3) . . ? I3 I1 I2 59.048(3) . . ? P1 Cu1 I4 106.062(17) . . ? P1 Cu1 I3 108.190(18) . . ? I4 Cu1 I3 115.631(11) . . ? P1 Cu1 I2 106.762(18) . . ? I4 Cu1 I2 111.168(10) . . ? I3 Cu1 I2 108.608(10) . . ? P1 Cu1 Cu2 142.74(2) . . ? I4 Cu1 Cu2 59.007(8) . . ? I3 Cu1 Cu2 108.977(11) . . ? I2 Cu1 Cu2 58.161(8) . . ? P1 Cu1 Cu4 138.95(2) . . ? I4 Cu1 Cu4 59.124(9) . . ? I3 Cu1 Cu4 59.078(9) . . ? I2 Cu1 Cu4 114.290(11) . . ? Cu2 Cu1 Cu4 66.603(10) . . ? P1 Cu1 Cu3 146.511(19) . . ? I4 Cu1 Cu3 107.307(11) . . ? I3 Cu1 Cu3 58.680(8) . . ? I2 Cu1 Cu3 57.797(8) . . ? Cu2 Cu1 Cu3 58.659(9) . . ? Cu4 Cu1 Cu3 64.710(10) . . ? P4 Cu4 I4 106.692(18) . . ? P4 Cu4 I3 117.043(19) . . ? I4 Cu4 I3 112.621(11) . . ? P4 Cu4 I1 110.414(17) . . ? I4 Cu4 I1 103.411(10) . . ? I3 Cu4 I1 105.844(10) . . ? P4 Cu4 Cu1 146.284(19) . . ? I4 Cu4 Cu1 57.396(8) . . ? I3 Cu4 Cu1 57.647(8) . . ? I1 Cu4 Cu1 102.562(11) . . ? P4 Cu4 Cu3 151.709(19) . . ? I4 Cu4 Cu3 100.744(11) . . ? I3 Cu4 Cu3 55.784(8) . . ? I1 Cu4 Cu3 55.242(8) . . ? Cu1 Cu4 Cu3 57.716(9) . . ? P4 Cu4 Cu2 142.576(19) . . ? I4 Cu4 Cu2 54.958(8) . . ? I3 Cu4 Cu2 100.379(11) . . ? I1 Cu4 Cu2 54.747(8) . . ? Cu1 Cu4 Cu2 56.650(9) . . ? Cu3 Cu4 Cu2 53.707(9) . . ? P2 Cu2 I2 108.165(18) . . ? P2 Cu2 I1 107.713(18) . . ? I2 Cu2 I1 114.718(11) . . ? P2 Cu2 I4 111.339(17) . . ? I2 Cu2 I4 110.615(10) . . ? I1 Cu2 I4 104.269(11) . . ? P2 Cu2 Cu3 140.709(19) . . ? I2 Cu2 Cu3 58.826(9) . . ? I1 Cu2 Cu3 58.675(9) . . ? I4 Cu2 Cu3 107.848(11) . . ? P2 Cu2 Cu1 148.915(19) . . ? I2 Cu2 Cu1 59.043(8) . . ? I1 Cu2 Cu1 103.293(11) . . ? I4 Cu2 Cu1 57.503(8) . . ? Cu3 Cu2 Cu1 60.808(9) . . ? P2 Cu2 Cu4 145.033(19) . . ? I2 Cu2 Cu4 106.797(10) . . ? I1 Cu2 Cu4 55.512(8) . . ? I4 Cu2 Cu4 55.156(8) . . ? Cu3 Cu2 Cu4 61.774(10) . . ? Cu1 Cu2 Cu4 56.747(9) . . ? P3 Cu3 I1 110.758(18) . . ? P3 Cu3 I2 107.446(19) . . ? I1 Cu3 I2 115.761(11) . . ? P3 Cu3 I3 106.020(18) . . ? I1 Cu3 I3 107.524(11) . . ? I2 Cu3 I3 108.900(10) . . ? P3 Cu3 Cu2 144.17(2) . . ? I1 Cu3 Cu2 59.369(9) . . ? I2 Cu3 Cu2 59.234(9) . . ? I3 Cu3 Cu2 109.783(11) . . ? P3 Cu3 Cu1 145.355(19) . . ? I1 Cu3 Cu1 103.597(11) . . ? I2 Cu3 Cu1 59.072(9) . . ? I3 Cu3 Cu1 57.743(8) . . ? Cu2 Cu3 Cu1 60.533(9) . . ? P3 Cu3 Cu4 142.90(2) . . ? I1 Cu3 Cu4 56.646(8) . . ? I2 Cu3 Cu4 109.220(11) . . ? I3 Cu3 Cu4 56.231(8) . . ? Cu2 Cu3 Cu4 64.519(10) . . ? Cu1 Cu3 Cu4 57.574(9) . . ? C13 P1 C7 103.15(10) . . ? C13 P1 C1 105.75(10) . . ? C7 P1 C1 105.15(10) . . ? C13 P1 Cu1 110.95(7) . . ? C7 P1 Cu1 117.17(8) . . ? C1 P1 Cu1 113.58(7) . . ? C67 P4 C61 104.19(11) . . ? C67 P4 C55 104.12(11) . . ? C61 P4 C55 101.29(10) . . ? C67 P4 Cu4 112.81(8) . . ? C61 P4 Cu4 116.21(8) . . ? C55 P4 Cu4 116.57(8) . . ? C19 P2 C31 104.42(10) . . ? C19 P2 C25 101.25(10) . . ? C31 P2 C25 105.29(10) . . ? C19 P2 Cu2 116.50(8) . . ? C31 P2 Cu2 112.87(7) . . ? C25 P2 Cu2 115.07(7) . . ? C43 P3 C37 104.77(10) . . ? C43 P3 C49 103.55(10) . . ? C37 P3 C49 104.04(10) . . ? C43 P3 Cu3 115.50(7) . . ? C37 P3 Cu3 114.21(7) . . ? C49 P3 Cu3 113.46(7) . . ? C9 C10 C11 120.2(2) . . ? C59 C58 C57 120.1(2) . . ? C10 C9 C8 120.3(2) . . ? C58 C57 C56 120.3(2) . . ? C10 C11 C12 119.9(2) . . ? C58 C59 C60 119.6(2) . . ? C9 C8 C7 120.4(2) . . ? C55 C56 C57 120.3(2) . . ? C7 C12 C11 120.7(2) . . ? C4 C5 C6 120.4(2) . . ? C12 C7 C8 118.6(2) . . ? C12 C7 P1 118.75(16) . . ? C8 C7 P1 122.62(18) . . ? C59 C60 C55 121.0(2) . . ? C1 C6 C5 120.2(2) . . ? C56 C55 C60 118.6(2) . . ? C56 C55 P4 123.74(18) . . ? C60 C55 P4 117.52(18) . . ? C70 C69 C68 120.3(3) . . ? C69 C68 C67 120.7(3) . . ? C3 C4 C5 119.8(2) . . ? C71 C70 C69 119.3(3) . . ? C6 C1 C2 118.7(2) . . ? C6 C1 P1 123.66(18) . . ? C2 C1 P1 117.58(16) . . ? C68 C67 C72 118.6(2) . . ? C68 C67 P4 120.47(18) . . ? C72 C67 P4 120.80(19) . . ? C61 C66 C65 120.3(3) . . ? C14 C13 C18 118.5(2) . . ? C14 C13 P1 122.47(18) . . ? C18 C13 P1 118.49(18) . . ? C17 C18 C13 120.5(2) . . ? C4 C3 C2 120.2(2) . . ? C70 C71 C72 120.7(3) . . ? C64 C65 C66 120.7(3) . . ? C16 C17 C18 120.6(2) . . ? C13 C14 C15 120.7(2) . . ? C3 C2 C1 120.6(2) . . ? C71 C72 C67 120.3(3) . . ? C66 C61 C62 118.7(2) . . ? C66 C61 P4 121.86(19) . . ? C62 C61 P4 119.33(19) . . ? C16 C15 C14 120.4(3) . . ? C17 C16 C15 119.3(2) . . ? C63 C64 C65 119.7(2) . . ? C61 C62 C63 120.3(3) . . ? C64 C63 C62 120.4(3) . . ? C34 C33 C32 120.6(2) . . ? C22 C23 C24 120.3(3) . . ? C51 C52 C53 119.9(2) . . ? C33 C34 C35 120.0(2) . . ? C19 C24 C23 120.2(2) . . ? C52 C51 C50 120.4(3) . . ? C52 C53 C54 120.2(3) . . ? C33 C32 C31 120.4(2) . . ? C34 C35 C36 119.8(2) . . ? C53 C54 C49 120.5(3) . . ? C21 C22 C23 120.3(2) . . ? C32 C31 C36 118.5(2) . . ? C32 C31 P2 122.33(19) . . ? C36 C31 P2 118.97(17) . . ? C49 C50 C51 120.1(2) . . ? C35 C36 C31 120.7(2) . . ? C54 C49 C50 118.9(2) . . ? C54 C49 P3 117.91(18) . . ? C50 C49 P3 123.12(18) . . ? C24 C19 C20 119.0(2) . . ? C24 C19 P2 119.67(17) . . ? C20 C19 P2 121.38(18) . . ? C41 C42 C37 120.6(2) . . ? C42 C41 C40 119.6(2) . . ? C22 C21 C20 120.1(2) . . ? C21 C20 C19 120.3(2) . . ? C38 C37 C42 119.0(2) . . ? C38 C37 P3 123.96(18) . . ? C42 C37 P3 117.00(16) . . ? C39 C40 C41 120.4(2) . . ? C26 C25 C30 118.5(2) . . ? C26 C25 P2 124.41(17) . . ? C30 C25 P2 117.07(17) . . ? C44 C43 C48 118.9(2) . . ? C44 C43 P3 118.76(17) . . ? C48 C43 P3 122.29(17) . . ? C39 C38 C37 120.4(2) . . ? C40 C39 C38 120.0(2) . . ? C29 C30 C25 120.6(2) . . ? C45 C44 C43 120.6(2) . . ? C25 C26 C27 120.7(2) . . ? C47 C48 C43 120.3(2) . . ? C46 C45 C44 119.8(2) . . ? C28 C29 C30 120.2(2) . . ? C28 C27 C26 120.3(2) . . ? C48 C47 C46 120.1(2) . . ? C47 C46 C45 120.3(2) . . ? C27 C28 C29 119.6(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.308 _refine_diff_density_min -1.042 _refine_diff_density_rms 0.141 data_cuipph_mono_077k _database_code_depnum_ccdc_archive 'CCDC 777572' #TrackingRef 'mono-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method chloroform/ether _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 77(1) _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 0.0007 0.0011 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' H H 0.0000 0.0000 'International Tables Vol C Tables 6.1.1.4' Cu Cu 0.2733 0.9097 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' I I -1.0407 1.3054 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' P P 0.0618 0.0648 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 13.4031(3) _cell_length_b 26.3883(5) _cell_length_c 19.3872(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.305(7) _cell_angle_gamma 90.00 _cell_volume 6766.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 77(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 1.84 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8407 _exptl_absorpt_correction_T_max 0.9480 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.5886 _diffrn_source 'SPring-8 BL02B1 bending magnet' _diffrn_source_type 'SPring-8 beamline BL02B1' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'SPring-8 BL02B1 Large cylindrical Image-Plate camera' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 110090 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 24.49 _reflns_number_total 19775 _reflns_number_gt 14623 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_cell_refinement 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2008), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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. Anomalous dispersion parameters are taken from S. Sasaki, KEK Report 88-14, 1-136 (1989). ; _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^)+(0.0106P)^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 19775 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0178 _refine_ls_wR_factor_ref 0.0315 _refine_ls_wR_factor_gt 0.0312 _refine_ls_goodness_of_fit_ref 0.749 _refine_ls_restrained_S_all 0.749 _refine_ls_shift/su_max 0.002 _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 I4 I 0.489291(8) -0.200944(4) 0.341812(6) 0.01486(2) Uani 1 1 d . . . I3 I 0.180321(8) -0.195427(4) 0.212933(7) 0.01667(3) Uani 1 1 d . . . I2 I 0.440164(8) -0.138907(4) 0.127948(6) 0.01521(3) Uani 1 1 d . . . I1 I 0.328676(9) -0.062481(4) 0.309186(7) 0.01697(3) Uani 1 1 d . . . Cu1 Cu 0.377772(16) -0.206478(8) 0.216626(12) 0.01643(5) Uani 1 1 d . . . Cu4 Cu 0.301214(16) -0.162622(8) 0.328911(12) 0.01832(5) Uani 1 1 d . . . Cu2 Cu 0.475317(15) -0.116236(8) 0.264296(12) 0.01607(5) Uani 1 1 d . . . Cu3 Cu 0.283423(16) -0.112065(8) 0.188770(12) 0.01757(5) Uani 1 1 d . . . P1 P 0.40565(3) -0.284078(17) 0.17536(3) 0.01407(9) Uani 1 1 d . . . P4 P 0.24747(3) -0.176074(17) 0.43191(3) 0.01746(10) Uani 1 1 d . . . P2 P 0.61873(3) -0.070381(17) 0.28561(2) 0.01417(9) Uani 1 1 d . . . P3 P 0.17819(3) -0.066101(17) 0.11069(3) 0.01531(9) Uani 1 1 d . . . C10 C 0.24434(13) -0.41698(7) 0.26547(11) 0.0243(4) Uani 1 1 d . . . H10 H 0.2119 -0.4443 0.2849 0.029 Uiso 1 1 calc R . . C58 C 0.08164(15) -0.32713(7) 0.45300(12) 0.0312(5) Uani 1 1 d . . . H58 H 0.0448 -0.3575 0.4566 0.037 Uiso 1 1 calc R . . C9 C 0.27607(14) -0.42259(7) 0.20159(11) 0.0260(5) Uani 1 1 d . . . H9 H 0.2648 -0.4537 0.1769 0.031 Uiso 1 1 calc R . . C57 C 0.13607(14) -0.30539(7) 0.51202(11) 0.0278(5) Uani 1 1 d . . . H57 H 0.1372 -0.3211 0.5562 0.033 Uiso 1 1 calc R . . C11 C 0.25986(14) -0.37160(7) 0.30104(11) 0.0249(4) Uani 1 1 d . . . H11 H 0.2375 -0.3676 0.3448 0.030 Uiso 1 1 calc R . . C59 C 0.08083(16) -0.30467(8) 0.38884(12) 0.0324(5) Uani 1 1 d . . . H59 H 0.0436 -0.3196 0.3481 0.039 Uiso 1 1 calc R . . C8 C 0.32406(13) -0.38320(7) 0.17348(11) 0.0221(4) Uani 1 1 d . . . H8 H 0.3454 -0.3874 0.1294 0.026 Uiso 1 1 calc R . . C56 C 0.18914(14) -0.26078(7) 0.50736(11) 0.0240(4) Uani 1 1 d . . . H56 H 0.2260 -0.2460 0.5484 0.029 Uiso 1 1 calc R . . C12 C 0.30803(13) -0.33186(7) 0.27301(10) 0.0195(4) Uani 1 1 d . . . H12 H 0.3182 -0.3007 0.2977 0.023 Uiso 1 1 calc R . . C5 C 0.67677(15) -0.36177(8) 0.20994(14) 0.0461(7) Uani 1 1 d . . . H5 H 0.6995 -0.3957 0.2180 0.055 Uiso 1 1 calc R . . C7 C 0.34166(12) -0.33720(6) 0.20919(10) 0.0156(4) Uani 1 1 d . . . C60 C 0.13453(15) -0.26005(7) 0.38354(11) 0.0274(5) Uani 1 1 d . . . H60 H 0.1342 -0.2449 0.3391 0.033 Uiso 1 1 calc R . . C6 C 0.57382(14) -0.35100(7) 0.20121(12) 0.0326(5) Uani 1 1 d . . . H6 H 0.5268 -0.3776 0.2039 0.039 Uiso 1 1 calc R . . C55 C 0.18864(13) -0.23754(7) 0.44283(10) 0.0194(4) Uani 1 1 d . . . C69 C 0.49220(15) -0.20894(9) 0.58036(12) 0.0372(6) Uani 1 1 d . . . H69 H 0.5340 -0.2376 0.5936 0.045 Uiso 1 1 calc R . . C68 C 0.41195(14) -0.21286(8) 0.52594(11) 0.0282(5) Uani 1 1 d . . . H68 H 0.3997 -0.2440 0.5015 0.034 Uiso 1 1 calc R . . C4 C 0.74601(15) -0.32334(8) 0.20698(13) 0.0378(6) Uani 1 1 d . . . H4 H 0.8162 -0.3308 0.2123 0.045 Uiso 1 1 calc R . . C70 C 0.51184(16) -0.16386(10) 0.61545(12) 0.0427(6) Uani 1 1 d . . . H70 H 0.5667 -0.1613 0.6530 0.051 Uiso 1 1 calc R . . C1 C 0.53929(13) -0.30192(7) 0.18864(10) 0.0179(4) Uani 1 1 d . . . C67 C 0.34898(13) -0.17168(7) 0.50655(10) 0.0201(4) Uani 1 1 d . . . C66 C 0.11602(17) -0.13472(8) 0.51698(13) 0.0402(6) Uani 1 1 d . . . H66 H 0.1459 -0.1578 0.5519 0.048 Uiso 1 1 calc R . . C13 C 0.36302(13) -0.28765(6) 0.08195(10) 0.0162(4) Uani 1 1 d . . . C18 C 0.26042(14) -0.29456(8) 0.05793(11) 0.0294(5) Uani 1 1 d . . . H18 H 0.2162 -0.3009 0.0906 0.035 Uiso 1 1 calc R . . C3 C 0.71291(14) -0.27429(7) 0.19633(11) 0.0274(5) Uani 1 1 d . . . H3 H 0.7604 -0.2477 0.1952 0.033 Uiso 1 1 calc R . . C71 C 0.45139(17) -0.12243(10) 0.59572(12) 0.0422(6) Uani 1 1 d . . . H71 H 0.4651 -0.0911 0.6195 0.051 Uiso 1 1 calc R . . C65 C 0.03760(18) -0.10325(8) 0.52947(15) 0.0491(7) Uani 1 1 d . . . H65 H 0.0130 -0.1055 0.5726 0.059 Uiso 1 1 calc R . . C17 C 0.22157(15) -0.29244(8) -0.01243(11) 0.0328(5) Uani 1 1 d . . . H17 H 0.1514 -0.2978 -0.0278 0.039 Uiso 1 1 calc R . . C14 C 0.42527(15) -0.27738(8) 0.03340(11) 0.0278(5) Uani 1 1 d . . . H14 H 0.4955 -0.2720 0.0486 0.033 Uiso 1 1 calc R . . C2 C 0.61019(13) -0.26337(7) 0.18725(10) 0.0217(4) Uani 1 1 d . . . H2 H 0.5880 -0.2293 0.1800 0.026 Uiso 1 1 calc R . . C72 C 0.37045(15) -0.12629(8) 0.54121(11) 0.0307(5) Uani 1 1 d . . . H72 H 0.3296 -0.0974 0.5277 0.037 Uiso 1 1 calc R . . C61 C 0.15055(13) -0.13228(7) 0.45320(11) 0.0211(4) Uani 1 1 d . . . C15 C 0.38628(17) -0.27491(9) -0.03716(11) 0.0382(6) Uani 1 1 d . . . H15 H 0.4300 -0.2679 -0.0699 0.046 Uiso 1 1 calc R . . C16 C 0.28449(16) -0.28260(8) -0.06033(11) 0.0311(5) Uani 1 1 d . . . H16 H 0.2582 -0.2811 -0.1088 0.037 Uiso 1 1 calc R . . C64 C -0.00444(15) -0.06898(8) 0.48006(13) 0.0358(6) Uani 1 1 d . . . H64 H -0.0578 -0.0476 0.4891 0.043 Uiso 1 1 calc R . . C62 C 0.10754(14) -0.09773(7) 0.40404(11) 0.0267(5) Uani 1 1 d . . . H62 H 0.1306 -0.0957 0.3603 0.032 Uiso 1 1 calc R . . C63 C 0.03049(15) -0.06561(8) 0.41783(12) 0.0335(5) Uani 1 1 d . . . H63 H 0.0023 -0.0414 0.3839 0.040 Uiso 1 1 calc R . . C33 C 0.88517(14) -0.14958(7) 0.29448(12) 0.0286(5) Uani 1 1 d . . . H33 H 0.9380 -0.1615 0.3294 0.034 Uiso 1 1 calc R . . C23 C 0.64660(19) -0.05674(9) 0.49729(12) 0.0451(6) Uani 1 1 d . . . H23 H 0.6178 -0.0723 0.5337 0.054 Uiso 1 1 calc R . . C52 C -0.01129(17) -0.16720(7) -0.05510(12) 0.0349(6) Uani 1 1 d . . . H52 H -0.0493 -0.1883 -0.0894 0.042 Uiso 1 1 calc R . . C34 C 0.88692(14) -0.16062(7) 0.22546(12) 0.0292(5) Uani 1 1 d . . . H34 H 0.9414 -0.1796 0.2127 0.035 Uiso 1 1 calc R . . C24 C 0.61769(16) -0.07223(8) 0.42898(11) 0.0317(5) Uani 1 1 d . . . H24 H 0.5690 -0.0985 0.4187 0.038 Uiso 1 1 calc R . . C51 C -0.05987(16) -0.13531(8) -0.01536(11) 0.0316(5) Uani 1 1 d . . . H51 H -0.1317 -0.1347 -0.0220 0.038 Uiso 1 1 calc R . . C53 C 0.09312(18) -0.16841(8) -0.04483(12) 0.0400(6) Uani 1 1 d . . . H53 H 0.1270 -0.1905 -0.0721 0.048 Uiso 1 1 calc R . . C32 C 0.80680(13) -0.12115(7) 0.31382(11) 0.0217(4) Uani 1 1 d . . . H32 H 0.8068 -0.1133 0.3617 0.026 Uiso 1 1 calc R . . C35 C 0.80920(14) -0.14408(7) 0.17445(11) 0.0265(5) Uani 1 1 d . . . H35 H 0.8104 -0.1514 0.1266 0.032 Uiso 1 1 calc R . . C54 C 0.14873(16) -0.13756(8) 0.00503(11) 0.0326(5) Uani 1 1 d . . . H54 H 0.2205 -0.1389 0.0122 0.039 Uiso 1 1 calc R . . C22 C 0.71713(17) -0.01879(8) 0.51267(12) 0.0364(6) Uani 1 1 d . . . H22 H 0.7369 -0.0082 0.5597 0.044 Uiso 1 1 calc R . . C31 C 0.72808(12) -0.10407(6) 0.26309(10) 0.0162(4) Uani 1 1 d . . . C50 C -0.00512(14) -0.10410(7) 0.03430(11) 0.0244(4) Uani 1 1 d . . . H50 H -0.0396 -0.0822 0.0614 0.029 Uiso 1 1 calc R . . C36 C 0.72948(13) -0.11669(7) 0.19363(10) 0.0196(4) Uani 1 1 d . . . H36 H 0.6751 -0.1064 0.1587 0.024 Uiso 1 1 calc R . . C49 C 0.09959(14) -0.10448(6) 0.04481(10) 0.0196(4) Uani 1 1 d . . . C19 C 0.65899(13) -0.04987(6) 0.37512(10) 0.0170(4) Uani 1 1 d . . . C42 C 0.03754(13) -0.05215(7) 0.19787(10) 0.0224(4) Uani 1 1 d . . . H42 H 0.0527 -0.0864 0.2103 0.027 Uiso 1 1 calc R . . C41 C -0.03347(13) -0.02612(7) 0.22845(11) 0.0250(4) Uani 1 1 d . . . H41 H -0.0687 -0.0428 0.2606 0.030 Uiso 1 1 calc R . . C21 C 0.75897(15) 0.00377(7) 0.46021(11) 0.0284(5) Uani 1 1 d . . . H21 H 0.8078 0.0299 0.4710 0.034 Uiso 1 1 calc R . . C20 C 0.73009(13) -0.01155(7) 0.39199(11) 0.0226(4) Uani 1 1 d . . . H20 H 0.7591 0.0043 0.3559 0.027 Uiso 1 1 calc R . . C37 C 0.08715(12) -0.02825(6) 0.14875(9) 0.0151(4) Uani 1 1 d . . . C40 C -0.05312(13) 0.02446(7) 0.21200(11) 0.0238(4) Uani 1 1 d . . . H40 H -0.1011 0.0425 0.2336 0.029 Uiso 1 1 calc R . . C25 C 0.61505(12) -0.00998(6) 0.23901(9) 0.0151(4) Uani 1 1 d . . . C43 C 0.23868(13) -0.02145(6) 0.05925(10) 0.0162(4) Uani 1 1 d . . . C38 C 0.06590(13) 0.02214(7) 0.13244(10) 0.0190(4) Uani 1 1 d . . . H38 H 0.0991 0.0387 0.0990 0.023 Uiso 1 1 calc R . . C39 C -0.00344(13) 0.04853(7) 0.16452(11) 0.0235(4) Uani 1 1 d . . . H39 H -0.0166 0.0832 0.1537 0.028 Uiso 1 1 calc R . . C30 C 0.53827(13) 0.02390(7) 0.24753(10) 0.0213(4) Uani 1 1 d . . . H30 H 0.4893 0.0145 0.2755 0.026 Uiso 1 1 calc R . . C44 C 0.33722(13) -0.00597(7) 0.08468(10) 0.0199(4) Uani 1 1 d . . . H44 H 0.3707 -0.0183 0.1284 0.024 Uiso 1 1 calc R . . C26 C 0.68413(13) 0.00444(7) 0.19645(10) 0.0214(4) Uani 1 1 d . . . H26 H 0.7370 -0.0181 0.1898 0.026 Uiso 1 1 calc R . . C48 C 0.19044(14) -0.00229(7) -0.00425(10) 0.0218(4) Uani 1 1 d . . . H48 H 0.1233 -0.0125 -0.0221 0.026 Uiso 1 1 calc R . . C45 C 0.38648(15) 0.02739(7) 0.04631(11) 0.0258(5) Uani 1 1 d . . . H45 H 0.4541 0.0373 0.0634 0.031 Uiso 1 1 calc R . . C29 C 0.53249(14) 0.07098(7) 0.21575(11) 0.0239(4) Uani 1 1 d . . . H29 H 0.4806 0.0940 0.2230 0.029 Uiso 1 1 calc R . . C27 C 0.67708(14) 0.05144(7) 0.16345(11) 0.0251(4) Uani 1 1 d . . . H27 H 0.7243 0.0605 0.1340 0.030 Uiso 1 1 calc R . . C47 C 0.23957(14) 0.03160(7) -0.04171(10) 0.0253(4) Uani 1 1 d . . . H47 H 0.2058 0.0449 -0.0848 0.030 Uiso 1 1 calc R . . C46 C 0.33788(15) 0.04613(7) -0.01643(11) 0.0277(5) Uani 1 1 d . . . H46 H 0.3719 0.0691 -0.0424 0.033 Uiso 1 1 calc R . . C28 C 0.60171(14) 0.08484(7) 0.17347(10) 0.0233(4) Uani 1 1 d . . . H28 H 0.5973 0.1171 0.1515 0.028 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 I4 0.01220(5) 0.01548(5) 0.01582(6) 0.00142(5) -0.00093(4) 0.00088(4) I3 0.00966(5) 0.01708(6) 0.02237(7) 0.00105(5) -0.00010(5) -0.00143(4) I2 0.01328(6) 0.01605(5) 0.01614(6) 0.00042(5) 0.00195(4) 0.00133(5) I1 0.01608(6) 0.01262(5) 0.02257(7) -0.00222(5) 0.00417(5) 0.00103(5) Cu1 0.01379(11) 0.01482(11) 0.01988(12) -0.00186(9) 0.00033(9) 0.00030(9) Cu4 0.01601(11) 0.01684(11) 0.02238(13) -0.00101(10) 0.00395(9) -0.00035(9) Cu2 0.01194(11) 0.01562(11) 0.01994(13) -0.00072(9) 0.00045(9) -0.00133(8) Cu3 0.01259(11) 0.01791(11) 0.02124(13) 0.00244(9) -0.00019(9) 0.00237(9) P1 0.0101(2) 0.0139(2) 0.0179(3) -0.00052(18) 0.00121(18) -0.00069(17) P4 0.0148(2) 0.0145(2) 0.0243(3) -0.0023(2) 0.0069(2) -0.00124(18) P2 0.0119(2) 0.0148(2) 0.0153(2) -0.00045(18) 0.00038(18) -0.00126(18) P3 0.0120(2) 0.0152(2) 0.0178(3) 0.00062(19) -0.00025(18) 0.00135(18) C10 0.0167(10) 0.0232(10) 0.0331(12) 0.0091(9) 0.0046(9) -0.0037(8) C58 0.0319(12) 0.0193(10) 0.0453(15) 0.0012(10) 0.0147(11) -0.0079(9) C9 0.0245(11) 0.0189(10) 0.0344(13) -0.0011(9) 0.0038(9) -0.0067(8) C57 0.0269(11) 0.0235(10) 0.0345(13) 0.0099(9) 0.0090(9) 0.0001(9) C11 0.0203(10) 0.0313(11) 0.0243(12) 0.0060(9) 0.0075(8) 0.0010(8) C59 0.0393(13) 0.0254(11) 0.0354(13) -0.0088(10) 0.0145(10) -0.0132(10) C8 0.0209(10) 0.0214(10) 0.0250(11) -0.0030(8) 0.0072(8) -0.0025(8) C56 0.0199(10) 0.0233(10) 0.0288(12) 0.0015(9) 0.0045(8) 0.0008(8) C12 0.0159(9) 0.0193(9) 0.0224(11) -0.0007(8) 0.0003(8) 0.0005(7) C5 0.0210(12) 0.0258(11) 0.091(2) 0.0223(13) 0.0083(12) 0.0046(9) C7 0.0104(8) 0.0165(9) 0.0195(10) 0.0019(7) 0.0009(7) 0.0000(7) C60 0.0354(12) 0.0233(10) 0.0263(12) -0.0037(9) 0.0138(9) -0.0091(9) C6 0.0156(10) 0.0233(11) 0.0589(16) 0.0141(10) 0.0061(10) -0.0003(8) C55 0.0188(10) 0.0146(9) 0.0273(11) -0.0019(8) 0.0105(8) 0.0008(7) C69 0.0200(11) 0.0551(16) 0.0367(14) 0.0070(12) 0.0057(10) 0.0035(10) C68 0.0194(10) 0.0328(12) 0.0334(13) -0.0001(10) 0.0071(9) 0.0014(9) C4 0.0116(10) 0.0330(12) 0.0676(18) 0.0191(12) 0.0034(10) 0.0041(9) C70 0.0212(12) 0.0794(19) 0.0275(13) -0.0040(13) 0.0037(10) -0.0067(12) C1 0.0131(9) 0.0190(9) 0.0215(10) 0.0017(8) 0.0027(7) 0.0010(7) C67 0.0159(9) 0.0255(10) 0.0208(11) -0.0017(8) 0.0087(8) -0.0027(8) C66 0.0484(15) 0.0242(11) 0.0570(17) 0.0109(11) 0.0358(13) 0.0117(10) C13 0.0155(9) 0.0146(8) 0.0180(10) -0.0016(7) 0.0011(7) 0.0006(7) C18 0.0187(10) 0.0465(13) 0.0227(11) -0.0001(10) 0.0024(8) 0.0005(9) C3 0.0144(10) 0.0260(11) 0.0408(14) 0.0079(10) 0.0013(9) -0.0044(8) C71 0.0358(14) 0.0554(16) 0.0357(15) -0.0196(12) 0.0067(11) -0.0124(12) C65 0.0564(16) 0.0290(12) 0.075(2) 0.0088(13) 0.0513(15) 0.0106(11) C17 0.0225(11) 0.0456(14) 0.0271(12) -0.0015(10) -0.0055(9) 0.0021(10) C14 0.0215(10) 0.0391(12) 0.0232(12) -0.0035(9) 0.0049(9) -0.0083(9) C2 0.0157(9) 0.0175(9) 0.0309(12) 0.0031(8) 0.0012(8) -0.0005(7) C72 0.0283(12) 0.0335(12) 0.0304(13) -0.0089(10) 0.0051(9) -0.0030(9) C61 0.0138(9) 0.0145(9) 0.0367(12) -0.0071(8) 0.0095(8) -0.0043(7) C15 0.0420(14) 0.0543(15) 0.0202(12) -0.0032(11) 0.0110(10) -0.0138(12) C16 0.0408(13) 0.0323(12) 0.0179(11) -0.0031(9) -0.0024(9) -0.0005(10) C64 0.0183(11) 0.0260(11) 0.0665(18) -0.0121(12) 0.0170(11) 0.0004(9) C62 0.0170(10) 0.0326(11) 0.0282(12) -0.0098(9) -0.0027(8) 0.0024(8) C63 0.0222(11) 0.0337(12) 0.0406(14) -0.0109(11) -0.0067(10) 0.0062(9) C33 0.0136(10) 0.0175(10) 0.0516(15) 0.0019(10) -0.0041(9) -0.0006(8) C23 0.0665(17) 0.0502(15) 0.0191(12) -0.0030(11) 0.0085(11) -0.0223(13) C52 0.0474(14) 0.0188(10) 0.0313(13) -0.0002(9) -0.0155(10) -0.0044(10) C34 0.0141(10) 0.0174(10) 0.0582(16) -0.0049(10) 0.0122(10) -0.0011(8) C24 0.0415(13) 0.0312(12) 0.0219(12) -0.0040(9) 0.0038(10) -0.0154(10) C51 0.0276(11) 0.0294(11) 0.0336(13) 0.0031(10) -0.0079(9) -0.0098(9) C53 0.0519(15) 0.0259(12) 0.0356(14) -0.0124(10) -0.0125(11) 0.0141(11) C32 0.0161(9) 0.0194(9) 0.0282(12) 0.0025(8) -0.0006(8) -0.0025(8) C35 0.0228(11) 0.0227(10) 0.0374(13) -0.0057(9) 0.0147(9) -0.0048(8) C54 0.0277(11) 0.0320(12) 0.0346(13) -0.0099(10) -0.0060(9) 0.0096(9) C22 0.0528(15) 0.0339(13) 0.0194(12) -0.0104(10) -0.0041(10) 0.0004(11) C31 0.0106(9) 0.0128(8) 0.0251(11) 0.0018(7) 0.0029(7) -0.0032(7) C50 0.0214(10) 0.0232(10) 0.0272(12) 0.0004(9) -0.0002(8) -0.0033(8) C36 0.0162(9) 0.0179(9) 0.0251(11) -0.0006(8) 0.0044(8) -0.0008(7) C49 0.0234(10) 0.0139(9) 0.0190(10) 0.0014(7) -0.0045(8) 0.0001(7) C19 0.0162(9) 0.0159(9) 0.0175(10) -0.0016(7) -0.0015(7) 0.0014(7) C42 0.0177(10) 0.0206(10) 0.0289(12) 0.0041(8) 0.0031(8) -0.0003(8) C41 0.0168(10) 0.0315(11) 0.0282(12) 0.0028(9) 0.0082(8) -0.0009(8) C21 0.0311(12) 0.0179(10) 0.0316(13) -0.0054(9) -0.0085(9) 0.0002(8) C20 0.0212(10) 0.0193(9) 0.0249(11) 0.0012(8) -0.0029(8) -0.0001(8) C37 0.0087(8) 0.0175(9) 0.0177(10) -0.0013(7) -0.0019(7) -0.0012(7) C40 0.0157(10) 0.0262(10) 0.0303(12) -0.0070(9) 0.0062(8) 0.0019(8) C25 0.0144(9) 0.0144(8) 0.0152(9) 0.0005(7) -0.0015(7) -0.0001(7) C43 0.0160(9) 0.0158(9) 0.0173(10) -0.0016(7) 0.0041(7) 0.0028(7) C38 0.0183(9) 0.0184(9) 0.0203(10) 0.0008(8) 0.0035(8) -0.0017(7) C39 0.0211(10) 0.0177(9) 0.0313(12) -0.0025(8) 0.0035(9) 0.0023(8) C30 0.0172(10) 0.0192(9) 0.0282(12) 0.0005(8) 0.0059(8) -0.0021(7) C44 0.0198(10) 0.0177(9) 0.0205(10) 0.0001(8) -0.0013(8) -0.0012(7) C26 0.0185(10) 0.0192(9) 0.0275(11) 0.0031(8) 0.0072(8) 0.0025(8) C48 0.0181(10) 0.0270(10) 0.0200(11) -0.0004(8) 0.0020(8) 0.0017(8) C45 0.0228(11) 0.0265(10) 0.0275(12) -0.0012(9) 0.0019(9) -0.0067(8) C29 0.0197(10) 0.0177(9) 0.0343(12) 0.0012(8) 0.0044(9) 0.0033(8) C27 0.0230(10) 0.0240(10) 0.0300(12) 0.0070(9) 0.0096(9) 0.0004(8) C47 0.0287(11) 0.0318(11) 0.0156(10) 0.0029(9) 0.0038(8) 0.0031(9) C46 0.0310(12) 0.0286(11) 0.0245(12) 0.0033(9) 0.0080(9) -0.0073(9) C28 0.0233(10) 0.0177(9) 0.0270(12) 0.0051(8) -0.0017(8) -0.0008(8) _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 I4 Cu1 2.6406(3) . ? I4 Cu2 2.6831(3) . ? I4 Cu4 2.6899(2) . ? I4 I1 4.23609(17) . ? I4 I2 4.4070(3) . ? I4 I3 4.4797(3) . ? I3 Cu1 2.6519(2) . ? I3 Cu3 2.6791(3) . ? I3 Cu4 2.6930(3) . ? I3 I1 4.3062(2) . ? I3 I2 4.3502(2) . ? I2 Cu3 2.6658(3) . ? I2 Cu2 2.6767(3) . ? I2 Cu1 2.7017(3) . ? I2 I1 4.5105(3) . ? I1 Cu3 2.6593(3) . ? I1 Cu2 2.6806(3) . ? I1 Cu4 2.7038(3) . ? Cu1 P1 2.2515(5) . ? Cu1 Cu2 2.8006(3) . ? Cu1 Cu4 2.8024(4) . ? Cu1 Cu3 2.8066(3) . ? Cu4 P4 2.2577(6) . ? Cu4 Cu3 3.0015(4) . ? Cu4 Cu2 3.0754(3) . ? Cu2 P2 2.2523(5) . ? Cu2 Cu3 2.7483(3) . ? Cu3 P3 2.2498(5) . ? P1 C13 1.8111(19) . ? P1 C7 1.8200(17) . ? P1 C1 1.8296(17) . ? P4 C67 1.823(2) . ? P4 C55 1.8306(18) . ? P4 C61 1.8348(18) . ? P2 C19 1.8147(19) . ? P2 C31 1.8265(17) . ? P2 C25 1.8289(17) . ? P3 C43 1.8171(18) . ? P3 C37 1.8227(18) . ? P3 C49 1.8254(18) . ? C10 C11 1.381(3) . ? C10 C9 1.381(3) . ? C58 C59 1.376(3) . ? C58 C57 1.379(3) . ? C9 C8 1.380(2) . ? C57 C56 1.386(2) . ? C11 C12 1.388(2) . ? C59 C60 1.393(3) . ? C8 C7 1.398(2) . ? C56 C55 1.392(3) . ? C12 C7 1.391(2) . ? C5 C4 1.382(3) . ? C5 C6 1.392(3) . ? C60 C55 1.389(3) . ? C6 C1 1.384(2) . ? C69 C70 1.375(3) . ? C69 C68 1.383(3) . ? C68 C67 1.390(3) . ? C4 C3 1.373(3) . ? C70 C71 1.378(3) . ? C1 C2 1.395(2) . ? C67 C72 1.381(3) . ? C66 C61 1.390(3) . ? C66 C65 1.391(3) . ? C13 C14 1.382(3) . ? C13 C18 1.391(2) . ? C18 C17 1.380(3) . ? C3 C2 1.390(2) . ? C71 C72 1.390(3) . ? C65 C64 1.370(3) . ? C17 C16 1.376(3) . ? C14 C15 1.385(3) . ? C61 C62 1.376(3) . ? C15 C16 1.381(3) . ? C64 C63 1.366(3) . ? C62 C63 1.395(3) . ? C33 C34 1.373(3) . ? C33 C32 1.391(3) . ? C23 C22 1.376(3) . ? C23 C24 1.380(3) . ? C52 C51 1.374(3) . ? C52 C53 1.382(3) . ? C34 C35 1.386(3) . ? C24 C19 1.390(3) . ? C51 C50 1.384(3) . ? C53 C54 1.386(3) . ? C32 C31 1.396(2) . ? C35 C36 1.389(2) . ? C54 C49 1.398(3) . ? C22 C21 1.374(3) . ? C31 C36 1.390(3) . ? C50 C49 1.385(2) . ? C19 C20 1.392(2) . ? C42 C41 1.383(2) . ? C42 C37 1.397(2) . ? C41 C40 1.388(3) . ? C21 C20 1.377(3) . ? C37 C38 1.386(2) . ? C40 C39 1.376(3) . ? C25 C26 1.389(2) . ? C25 C30 1.393(2) . ? C43 C48 1.390(2) . ? C43 C44 1.394(2) . ? C38 C39 1.387(2) . ? C30 C29 1.384(2) . ? C44 C45 1.387(3) . ? C26 C27 1.392(2) . ? C48 C47 1.384(3) . ? C45 C46 1.375(3) . ? C29 C28 1.383(3) . ? C27 C28 1.378(2) . ? C47 C46 1.384(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I4 Cu2 63.474(7) . . ? Cu1 I4 Cu4 63.426(9) . . ? Cu2 I4 Cu4 69.832(8) . . ? Cu1 I4 I1 73.261(6) . . ? Cu2 I4 I1 37.816(6) . . ? Cu4 I4 I1 38.360(5) . . ? Cu1 I4 I2 34.871(6) . . ? Cu2 I4 I2 34.644(5) . . ? Cu4 I4 I2 77.153(8) . . ? I1 I4 I2 62.877(4) . . ? Cu1 I4 I3 32.253(6) . . ? Cu2 I4 I3 71.700(6) . . ? Cu4 I4 I3 33.698(6) . . ? I1 I4 I3 59.139(3) . . ? I2 I4 I3 58.611(6) . . ? Cu1 I3 Cu3 63.532(7) . . ? Cu1 I3 Cu4 63.238(9) . . ? Cu3 I3 Cu4 67.934(8) . . ? Cu1 I3 I1 71.882(6) . . ? Cu3 I3 I1 36.075(6) . . ? Cu4 I3 I1 37.154(5) . . ? Cu1 I3 I2 36.037(6) . . ? Cu3 I3 I2 35.421(5) . . ? Cu4 I3 I2 78.203(7) . . ? I1 I3 I2 62.803(4) . . ? Cu1 I3 I4 32.099(6) . . ? Cu3 I3 I4 70.596(6) . . ? Cu4 I3 I4 33.654(6) . . ? I1 I3 I4 57.611(4) . . ? I2 I3 I4 59.860(4) . . ? Cu3 I2 Cu2 61.918(9) . . ? Cu3 I2 Cu1 63.048(8) . . ? Cu2 I2 Cu1 62.759(8) . . ? Cu3 I2 I3 35.624(5) . . ? Cu2 I2 I3 74.125(8) . . ? Cu1 I2 I3 35.272(6) . . ? Cu3 I2 I4 72.007(8) . . ? Cu2 I2 I4 34.739(6) . . ? Cu1 I2 I4 33.972(6) . . ? I3 I2 I4 61.529(6) . . ? Cu3 I2 I1 32.069(6) . . ? Cu2 I2 I1 32.683(5) . . ? Cu1 I2 I1 67.899(7) . . ? I3 I2 I1 58.122(5) . . ? I4 I2 I1 56.709(4) . . ? Cu3 I1 Cu2 61.950(8) . . ? Cu3 I1 Cu4 68.059(8) . . ? Cu2 I1 Cu4 69.663(7) . . ? Cu3 I1 I4 75.224(7) . . ? Cu2 I1 I4 37.857(6) . . ? Cu4 I1 I4 38.129(5) . . ? Cu3 I1 I3 36.385(6) . . ? Cu2 I1 I3 74.908(6) . . ? Cu4 I1 I3 36.982(6) . . ? I4 I1 I3 63.250(4) . . ? Cu3 I1 I2 32.156(5) . . ? Cu2 I1 I2 32.629(6) . . ? Cu4 I1 I2 75.108(6) . . ? I4 I1 I2 60.414(4) . . ? I3 I1 I2 59.075(4) . . ? P1 Cu1 I4 105.967(15) . . ? P1 Cu1 I3 108.218(14) . . ? I4 Cu1 I3 115.648(11) . . ? P1 Cu1 I2 106.733(15) . . ? I4 Cu1 I2 111.157(9) . . ? I3 Cu1 I2 108.690(9) . . ? P1 Cu1 Cu2 142.669(15) . . ? I4 Cu1 Cu2 59.003(7) . . ? I3 Cu1 Cu2 109.025(9) . . ? I2 Cu1 Cu2 58.184(8) . . ? P1 Cu1 Cu4 138.958(16) . . ? I4 Cu1 Cu4 59.145(8) . . ? I3 Cu1 Cu4 59.097(9) . . ? I2 Cu1 Cu4 114.308(10) . . ? Cu2 Cu1 Cu4 66.581(8) . . ? P1 Cu1 Cu3 146.559(17) . . ? I4 Cu1 Cu3 107.352(9) . . ? I3 Cu1 Cu3 58.705(7) . . ? I2 Cu1 Cu3 57.852(7) . . ? Cu2 Cu1 Cu3 58.699(8) . . ? Cu4 Cu1 Cu3 64.704(9) . . ? P4 Cu4 I4 106.671(16) . . ? P4 Cu4 I3 116.933(16) . . ? I4 Cu4 I3 112.649(10) . . ? P4 Cu4 I1 110.424(15) . . ? I4 Cu4 I1 103.511(8) . . ? I3 Cu4 I1 105.865(9) . . ? P4 Cu4 Cu1 146.238(16) . . ? I4 Cu4 Cu1 57.428(8) . . ? I3 Cu4 Cu1 57.665(8) . . ? I1 Cu4 Cu1 102.617(9) . . ? P4 Cu4 Cu3 151.697(16) . . ? I4 Cu4 Cu3 100.799(10) . . ? I3 Cu4 Cu3 55.812(8) . . ? I1 Cu4 Cu3 55.268(7) . . ? Cu1 Cu4 Cu3 57.716(8) . . ? P4 Cu4 Cu2 142.604(16) . . ? I4 Cu4 Cu2 54.980(6) . . ? I3 Cu4 Cu2 100.462(10) . . ? I1 Cu4 Cu2 54.814(6) . . ? Cu1 Cu4 Cu2 56.682(8) . . ? Cu3 Cu4 Cu2 53.761(8) . . ? P2 Cu2 I2 108.059(16) . . ? P2 Cu2 I1 107.755(14) . . ? I2 Cu2 I1 114.688(10) . . ? P2 Cu2 I4 111.383(15) . . ? I2 Cu2 I4 110.617(9) . . ? I1 Cu2 I4 104.327(9) . . ? P2 Cu2 Cu3 140.680(16) . . ? I2 Cu2 Cu3 58.847(9) . . ? I1 Cu2 Cu3 58.645(7) . . ? I4 Cu2 Cu3 107.838(9) . . ? P2 Cu2 Cu1 148.911(15) . . ? I2 Cu2 Cu1 59.058(8) . . ? I1 Cu2 Cu1 103.263(9) . . ? I4 Cu2 Cu1 57.523(8) . . ? Cu3 Cu2 Cu1 60.759(8) . . ? P2 Cu2 Cu4 145.120(16) . . ? I2 Cu2 Cu4 106.816(10) . . ? I1 Cu2 Cu4 55.523(7) . . ? I4 Cu2 Cu4 55.188(7) . . ? Cu3 Cu2 Cu4 61.745(8) . . ? Cu1 Cu2 Cu4 56.737(8) . . ? P3 Cu3 I1 110.767(16) . . ? P3 Cu3 I2 107.387(16) . . ? I1 Cu3 I2 115.775(10) . . ? P3 Cu3 I3 105.982(15) . . ? I1 Cu3 I3 107.540(10) . . ? I2 Cu3 I3 108.955(9) . . ? P3 Cu3 Cu2 144.189(16) . . ? I1 Cu3 Cu2 59.405(9) . . ? I2 Cu3 Cu2 59.236(8) . . ? I3 Cu3 Cu2 109.797(9) . . ? P3 Cu3 Cu1 145.287(16) . . ? I1 Cu3 Cu1 103.658(10) . . ? I2 Cu3 Cu1 59.101(7) . . ? I3 Cu3 Cu1 57.763(7) . . ? Cu2 Cu3 Cu1 60.542(8) . . ? P3 Cu3 Cu4 142.946(16) . . ? I1 Cu3 Cu4 56.674(8) . . ? I2 Cu3 Cu4 109.229(10) . . ? I3 Cu3 Cu4 56.254(8) . . ? Cu2 Cu3 Cu4 64.494(10) . . ? Cu1 Cu3 Cu4 57.580(8) . . ? C13 P1 C7 103.26(8) . . ? C13 P1 C1 105.71(8) . . ? C7 P1 C1 105.00(8) . . ? C13 P1 Cu1 111.03(6) . . ? C7 P1 Cu1 117.23(6) . . ? C1 P1 Cu1 113.51(6) . . ? C67 P4 C55 104.17(9) . . ? C67 P4 C61 104.25(9) . . ? C55 P4 C61 101.43(8) . . ? C67 P4 Cu4 112.84(6) . . ? C55 P4 Cu4 116.52(6) . . ? C61 P4 Cu4 116.02(7) . . ? C19 P2 C31 104.35(8) . . ? C19 P2 C25 101.10(8) . . ? C31 P2 C25 105.35(8) . . ? C19 P2 Cu2 116.66(6) . . ? C31 P2 Cu2 112.87(6) . . ? C25 P2 Cu2 115.06(6) . . ? C43 P3 C37 104.72(8) . . ? C43 P3 C49 103.53(9) . . ? C37 P3 C49 103.83(8) . . ? C43 P3 Cu3 115.60(6) . . ? C37 P3 Cu3 114.27(6) . . ? C49 P3 Cu3 113.56(6) . . ? C11 C10 C9 119.84(18) . . ? C59 C58 C57 119.78(19) . . ? C8 C9 C10 120.28(18) . . ? C58 C57 C56 120.5(2) . . ? C10 C11 C12 120.12(19) . . ? C58 C59 C60 120.1(2) . . ? C9 C8 C7 120.69(18) . . ? C57 C56 C55 120.31(19) . . ? C11 C12 C7 120.67(18) . . ? C4 C5 C6 120.28(19) . . ? C12 C7 C8 118.38(17) . . ? C12 C7 P1 118.81(14) . . ? C8 C7 P1 122.80(14) . . ? C55 C60 C59 120.5(2) . . ? C1 C6 C5 120.61(18) . . ? C60 C55 C56 118.76(17) . . ? C60 C55 P4 117.39(15) . . ? C56 C55 P4 123.68(15) . . ? C70 C69 C68 120.3(2) . . ? C69 C68 C67 120.7(2) . . ? C3 C4 C5 119.68(18) . . ? C69 C70 C71 119.5(2) . . ? C6 C1 C2 118.45(16) . . ? C6 C1 P1 123.89(14) . . ? C2 C1 P1 117.65(14) . . ? C72 C67 C68 118.48(19) . . ? C72 C67 P4 120.78(16) . . ? C68 C67 P4 120.51(15) . . ? C61 C66 C65 119.8(2) . . ? C14 C13 C18 118.09(18) . . ? C14 C13 P1 122.91(14) . . ? C18 C13 P1 118.47(14) . . ? C17 C18 C13 121.35(19) . . ? C4 C3 C2 120.26(18) . . ? C70 C71 C72 120.3(2) . . ? C64 C65 C66 120.6(2) . . ? C16 C17 C18 120.0(2) . . ? C13 C14 C15 120.61(19) . . ? C3 C2 C1 120.68(17) . . ? C67 C72 C71 120.6(2) . . ? C62 C61 C66 118.96(18) . . ? C62 C61 P4 119.60(16) . . ? C66 C61 P4 121.37(16) . . ? C16 C15 C14 120.6(2) . . ? C17 C16 C15 119.3(2) . . ? C63 C64 C65 120.0(2) . . ? C61 C62 C63 120.7(2) . . ? C64 C63 C62 120.0(2) . . ? C34 C33 C32 120.64(19) . . ? C22 C23 C24 120.0(2) . . ? C51 C52 C53 119.6(2) . . ? C33 C34 C35 119.95(18) . . ? C23 C24 C19 120.72(19) . . ? C52 C51 C50 120.6(2) . . ? C52 C53 C54 120.3(2) . . ? C33 C32 C31 120.14(19) . . ? C34 C35 C36 119.7(2) . . ? C53 C54 C49 120.2(2) . . ? C21 C22 C23 120.2(2) . . ? C36 C31 C32 118.56(17) . . ? C36 C31 P2 119.02(13) . . ? C32 C31 P2 122.22(15) . . ? C51 C50 C49 120.58(19) . . ? C35 C36 C31 121.00(18) . . ? C50 C49 C54 118.68(18) . . ? C50 C49 P3 123.73(15) . . ? C54 C49 P3 117.54(14) . . ? C24 C19 C20 118.21(18) . . ? C24 C19 P2 119.92(14) . . ? C20 C19 P2 121.87(15) . . ? C41 C42 C37 120.29(18) . . ? C42 C41 C40 119.84(18) . . ? C22 C21 C20 119.92(19) . . ? C21 C20 C19 120.95(19) . . ? C38 C37 C42 119.08(17) . . ? C38 C37 P3 124.05(14) . . ? C42 C37 P3 116.87(13) . . ? C39 C40 C41 120.23(18) . . ? C26 C25 C30 118.09(16) . . ? C26 C25 P2 124.39(13) . . ? C30 C25 P2 117.52(13) . . ? C48 C43 C44 119.02(17) . . ? C48 C43 P3 122.48(14) . . ? C44 C43 P3 118.50(14) . . ? C37 C38 C39 120.50(18) . . ? C40 C39 C38 120.02(18) . . ? C29 C30 C25 120.85(17) . . ? C45 C44 C43 120.15(18) . . ? C25 C26 C27 120.99(17) . . ? C47 C48 C43 120.47(18) . . ? C46 C45 C44 120.27(18) . . ? C28 C29 C30 120.45(17) . . ? C28 C27 C26 120.14(18) . . ? C46 C47 C48 119.98(19) . . ? C45 C46 C47 120.10(19) . . ? C27 C28 C29 119.46(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.944 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.076 data_cuipph_mono_045k _database_code_depnum_ccdc_archive 'CCDC 777573' #TrackingRef 'mono-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method chloroform/ether _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 45(1) _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 0.0007 0.0011 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' H H 0.0000 0.0000 'International Tables Vol C Tables 6.1.1.4' Cu Cu 0.2733 0.9097 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' I I -1.0407 1.3054 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' P P 0.0618 0.0648 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 13.3915(3) _cell_length_b 26.3236(5) _cell_length_c 19.3799(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.366(7) _cell_angle_gamma 90.00 _cell_volume 6740.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 45(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 1.85 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8402 _exptl_absorpt_correction_T_max 0.9479 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.5886 _diffrn_source 'SPring-8 BL02B1 bending magnet' _diffrn_source_type 'SPring-8 beamline BL02B1' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'SPring-8 BL02B1 Large cylindrical Image-Plate camera' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 109408 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 24.49 _reflns_number_total 19695 _reflns_number_gt 15416 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_cell_refinement 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2008), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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. Anomalous dispersion parameters are taken from S. Sasaki, KEK Report 88-14, 1-136 (1989). ; _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^)+(0.0124P)^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 19695 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0343 _refine_ls_wR_factor_gt 0.0341 _refine_ls_goodness_of_fit_ref 0.811 _refine_ls_restrained_S_all 0.811 _refine_ls_shift/su_max 0.003 _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 I4 I 0.490676(8) -0.201306(4) 0.341322(6) 0.00978(2) Uani 1 1 d . . . I3 I 0.181489(8) -0.196101(4) 0.211673(6) 0.01084(2) Uani 1 1 d . . . I2 I 0.441644(8) -0.139130(4) 0.127136(6) 0.00994(2) Uani 1 1 d . . . I1 I 0.329920(8) -0.062446(4) 0.308524(6) 0.01117(2) Uani 1 1 d . . . Cu1 Cu 0.379478(16) -0.206676(8) 0.215955(12) 0.01096(4) Uani 1 1 d . . . Cu4 Cu 0.302173(16) -0.162874(8) 0.327566(12) 0.01212(5) Uani 1 1 d . . . Cu2 Cu 0.476138(16) -0.116534(8) 0.263570(12) 0.01083(4) Uani 1 1 d . . . Cu3 Cu 0.284795(16) -0.112446(8) 0.188265(12) 0.01161(5) Uani 1 1 d . . . P1 P 0.40707(3) -0.284600(17) 0.17494(2) 0.00953(9) Uani 1 1 d . . . P4 P 0.24801(3) -0.176091(17) 0.43061(3) 0.01153(9) Uani 1 1 d . . . P2 P 0.61946(3) -0.070374(17) 0.28530(2) 0.00973(9) Uani 1 1 d . . . P3 P 0.17915(3) -0.066289(17) 0.11036(2) 0.01037(9) Uani 1 1 d . . . C10 C 0.24393(13) -0.41717(7) 0.26549(10) 0.0166(4) Uani 1 1 d . . . H10 H 0.2108 -0.4443 0.2849 0.020 Uiso 1 1 calc R . . C58 C 0.08174(15) -0.32749(7) 0.45210(11) 0.0215(4) Uani 1 1 d . . . H58 H 0.0445 -0.3578 0.4558 0.026 Uiso 1 1 calc R . . C9 C 0.27656(13) -0.42323(7) 0.20163(10) 0.0178(4) Uani 1 1 d . . . H9 H 0.2654 -0.4545 0.1771 0.021 Uiso 1 1 calc R . . C57 C 0.13790(14) -0.30603(7) 0.51126(11) 0.0190(4) Uani 1 1 d . . . H57 H 0.1399 -0.3220 0.5554 0.023 Uiso 1 1 calc R . . C11 C 0.25968(13) -0.37150(7) 0.30082(10) 0.0165(4) Uani 1 1 d . . . H11 H 0.2370 -0.3672 0.3444 0.020 Uiso 1 1 calc R . . C59 C 0.07987(15) -0.30478(7) 0.38772(11) 0.0210(4) Uani 1 1 d . . . H59 H 0.0420 -0.3197 0.3470 0.025 Uiso 1 1 calc R . . C8 C 0.32537(13) -0.38388(7) 0.17358(10) 0.0157(4) Uani 1 1 d . . . H8 H 0.3474 -0.3883 0.1298 0.019 Uiso 1 1 calc R . . C56 C 0.19127(13) -0.26137(7) 0.50634(10) 0.0164(4) Uani 1 1 d . . . H56 H 0.2295 -0.2469 0.5472 0.020 Uiso 1 1 calc R . . C12 C 0.30854(13) -0.33179(7) 0.27273(9) 0.0133(4) Uani 1 1 d . . . H12 H 0.3187 -0.3004 0.2971 0.016 Uiso 1 1 calc R . . C5 C 0.67812(15) -0.36319(8) 0.20769(12) 0.0272(5) Uani 1 1 d . . . H5 H 0.7008 -0.3972 0.2155 0.033 Uiso 1 1 calc R . . C7 C 0.34268(12) -0.33766(6) 0.20911(9) 0.0110(3) Uani 1 1 d . . . C60 C 0.13360(14) -0.25999(7) 0.38247(10) 0.0180(4) Uani 1 1 d . . . H60 H 0.1323 -0.2445 0.3381 0.022 Uiso 1 1 calc R . . C6 C 0.57517(14) -0.35218(7) 0.19965(11) 0.0203(4) Uani 1 1 d . . . H6 H 0.5280 -0.3788 0.2024 0.024 Uiso 1 1 calc R . . C55 C 0.18918(13) -0.23772(6) 0.44185(10) 0.0131(4) Uani 1 1 d . . . C69 C 0.49377(15) -0.20852(9) 0.57942(11) 0.0249(5) Uani 1 1 d . . . H69 H 0.5361 -0.2370 0.5926 0.030 Uiso 1 1 calc R . . C68 C 0.41369(14) -0.21264(7) 0.52448(10) 0.0186(4) Uani 1 1 d . . . H68 H 0.4025 -0.2437 0.4995 0.022 Uiso 1 1 calc R . . C4 C 0.74765(14) -0.32466(8) 0.20433(11) 0.0236(5) Uani 1 1 d . . . H4 H 0.8177 -0.3323 0.2088 0.028 Uiso 1 1 calc R . . C70 C 0.51233(15) -0.16335(9) 0.61496(11) 0.0275(5) Uani 1 1 d . . . H70 H 0.5672 -0.1607 0.6526 0.033 Uiso 1 1 calc R . . C1 C 0.54083(13) -0.30266(7) 0.18765(9) 0.0127(3) Uani 1 1 d . . . C67 C 0.34940(13) -0.17139(7) 0.50555(9) 0.0135(4) Uani 1 1 d . . . C66 C 0.11458(16) -0.13545(7) 0.51508(12) 0.0249(5) Uani 1 1 d . . . H66 H 0.1434 -0.1591 0.5497 0.030 Uiso 1 1 calc R . . C13 C 0.36337(13) -0.28811(6) 0.08138(9) 0.0115(3) Uani 1 1 d . . . C18 C 0.26094(14) -0.29619(8) 0.05761(10) 0.0197(4) Uani 1 1 d . . . H18 H 0.2173 -0.3035 0.0904 0.024 Uiso 1 1 calc R . . C3 C 0.71451(14) -0.27505(7) 0.19443(10) 0.0180(4) Uani 1 1 d . . . H3 H 0.7621 -0.2484 0.1934 0.022 Uiso 1 1 calc R . . C71 C 0.45067(15) -0.12183(9) 0.59562(11) 0.0273(5) Uani 1 1 d . . . H71 H 0.4636 -0.0905 0.6198 0.033 Uiso 1 1 calc R . . C65 C 0.03615(16) -0.10390(8) 0.52750(13) 0.0302(5) Uani 1 1 d . . . H65 H 0.0107 -0.1066 0.5703 0.036 Uiso 1 1 calc R . . C17 C 0.22128(15) -0.29382(8) -0.01277(10) 0.0219(4) Uani 1 1 d . . . H17 H 0.1513 -0.2999 -0.0281 0.026 Uiso 1 1 calc R . . C14 C 0.42538(14) -0.27635(7) 0.03276(10) 0.0185(4) Uani 1 1 d . . . H14 H 0.4954 -0.2702 0.0479 0.022 Uiso 1 1 calc R . . C2 C 0.61179(13) -0.26398(7) 0.18601(10) 0.0148(4) Uani 1 1 d . . . H2 H 0.5896 -0.2298 0.1791 0.018 Uiso 1 1 calc R . . C72 C 0.36986(15) -0.12582(8) 0.54084(10) 0.0201(4) Uani 1 1 d . . . H72 H 0.3283 -0.0971 0.5275 0.024 Uiso 1 1 calc R . . C61 C 0.15075(13) -0.13228(6) 0.45166(10) 0.0143(4) Uani 1 1 d . . . C15 C 0.38539(16) -0.27361(8) -0.03783(11) 0.0253(5) Uani 1 1 d . . . H15 H 0.4284 -0.2655 -0.0707 0.030 Uiso 1 1 calc R . . C16 C 0.28392(15) -0.28246(7) -0.06092(10) 0.0210(4) Uani 1 1 d . . . H16 H 0.2573 -0.2808 -0.1094 0.025 Uiso 1 1 calc R . . C64 C -0.00490(14) -0.06878(7) 0.47834(12) 0.0230(5) Uani 1 1 d . . . H64 H -0.0584 -0.0473 0.4873 0.028 Uiso 1 1 calc R . . C62 C 0.10902(13) -0.09702(7) 0.40251(10) 0.0176(4) Uani 1 1 d . . . H62 H 0.1330 -0.0947 0.3591 0.021 Uiso 1 1 calc R . . C63 C 0.03175(14) -0.06480(8) 0.41626(11) 0.0218(4) Uani 1 1 d . . . H63 H 0.0045 -0.0401 0.3827 0.026 Uiso 1 1 calc R . . C33 C 0.88603(14) -0.14985(7) 0.29590(11) 0.0200(4) Uani 1 1 d . . . H33 H 0.9385 -0.1617 0.3312 0.024 Uiso 1 1 calc R . . C23 C 0.64595(17) -0.05629(8) 0.49733(11) 0.0299(5) Uani 1 1 d . . . H23 H 0.6170 -0.0718 0.5337 0.036 Uiso 1 1 calc R . . C52 C -0.01111(16) -0.16742(7) -0.05580(11) 0.0231(5) Uani 1 1 d . . . H52 H -0.0492 -0.1885 -0.0902 0.028 Uiso 1 1 calc R . . C34 C 0.88883(14) -0.16118(7) 0.22673(12) 0.0208(4) Uani 1 1 d . . . H34 H 0.9434 -0.1804 0.2144 0.025 Uiso 1 1 calc R . . C24 C 0.61699(15) -0.07202(8) 0.42865(10) 0.0220(4) Uani 1 1 d . . . H24 H 0.5680 -0.0982 0.4182 0.026 Uiso 1 1 calc R . . C51 C -0.06009(15) -0.13517(7) -0.01617(11) 0.0214(4) Uani 1 1 d . . . H51 H -0.1319 -0.1344 -0.0230 0.026 Uiso 1 1 calc R . . C53 C 0.09340(16) -0.16899(8) -0.04529(11) 0.0260(5) Uani 1 1 d . . . H53 H 0.1271 -0.1913 -0.0724 0.031 Uiso 1 1 calc R . . C32 C 0.80752(13) -0.12131(7) 0.31462(10) 0.0156(4) Uani 1 1 d . . . H32 H 0.8070 -0.1135 0.3624 0.019 Uiso 1 1 calc R . . C35 C 0.81133(14) -0.14435(7) 0.17505(11) 0.0187(4) Uani 1 1 d . . . H35 H 0.8132 -0.1516 0.1273 0.022 Uiso 1 1 calc R . . C54 C 0.14937(15) -0.13807(7) 0.00475(11) 0.0221(4) Uani 1 1 d . . . H54 H 0.2212 -0.1396 0.0121 0.026 Uiso 1 1 calc R . . C22 C 0.71687(16) -0.01816(8) 0.51286(11) 0.0240(5) Uani 1 1 d . . . H22 H 0.7363 -0.0073 0.5599 0.029 Uiso 1 1 calc R . . C31 C 0.72923(12) -0.10406(6) 0.26342(10) 0.0115(3) Uani 1 1 d . . . C50 C -0.00484(13) -0.10379(7) 0.03365(10) 0.0165(4) Uani 1 1 d . . . H50 H -0.0392 -0.0816 0.0606 0.020 Uiso 1 1 calc R . . C36 C 0.73104(13) -0.11684(7) 0.19368(10) 0.0139(4) Uani 1 1 d . . . H36 H 0.6768 -0.1066 0.1585 0.017 Uiso 1 1 calc R . . C49 C 0.10041(13) -0.10465(6) 0.04442(9) 0.0135(4) Uani 1 1 d . . . C19 C 0.65927(13) -0.04968(6) 0.37511(9) 0.0120(4) Uani 1 1 d . . . C42 C 0.03792(13) -0.05261(7) 0.19720(10) 0.0154(4) Uani 1 1 d . . . H42 H 0.0529 -0.0870 0.2094 0.018 Uiso 1 1 calc R . . C41 C -0.03343(13) -0.02662(7) 0.22765(10) 0.0168(4) Uani 1 1 d . . . H41 H -0.0688 -0.0435 0.2596 0.020 Uiso 1 1 calc R . . C21 C 0.75951(15) 0.00413(7) 0.46025(10) 0.0190(4) Uani 1 1 d . . . H21 H 0.8088 0.0301 0.4711 0.023 Uiso 1 1 calc R . . C20 C 0.73088(13) -0.01119(7) 0.39178(10) 0.0152(4) Uani 1 1 d . . . H20 H 0.7601 0.0046 0.3557 0.018 Uiso 1 1 calc R . . C37 C 0.08815(12) -0.02844(6) 0.14850(9) 0.0105(3) Uani 1 1 d . . . C40 C -0.05343(13) 0.02425(7) 0.21145(10) 0.0165(4) Uani 1 1 d . . . H40 H -0.1019 0.0422 0.2327 0.020 Uiso 1 1 calc R . . C25 C 0.61568(13) -0.00986(6) 0.23852(9) 0.0108(3) Uani 1 1 d . . . C43 C 0.23944(13) -0.02137(6) 0.05892(9) 0.0110(3) Uani 1 1 d . . . C38 C 0.06728(13) 0.02225(7) 0.13241(9) 0.0130(4) Uani 1 1 d . . . H38 H 0.1010 0.0390 0.0994 0.016 Uiso 1 1 calc R . . C39 C -0.00273(13) 0.04861(7) 0.16444(10) 0.0158(4) Uani 1 1 d . . . H39 H -0.0157 0.0835 0.1539 0.019 Uiso 1 1 calc R . . C30 C 0.53886(13) 0.02416(7) 0.24728(10) 0.0144(4) Uani 1 1 d . . . H30 H 0.4901 0.0148 0.2755 0.017 Uiso 1 1 calc R . . C44 C 0.33870(13) -0.00613(7) 0.08428(10) 0.0139(4) Uani 1 1 d . . . H44 H 0.3724 -0.0187 0.1279 0.017 Uiso 1 1 calc R . . C26 C 0.68486(13) 0.00447(7) 0.19578(10) 0.0146(4) Uani 1 1 d . . . H26 H 0.7376 -0.0182 0.1890 0.018 Uiso 1 1 calc R . . C48 C 0.19074(13) -0.00188(7) -0.00445(10) 0.0151(4) Uani 1 1 d . . . H48 H 0.1234 -0.0120 -0.0222 0.018 Uiso 1 1 calc R . . C45 C 0.38810(14) 0.02735(7) 0.04598(10) 0.0175(4) Uani 1 1 d . . . H45 H 0.4560 0.0371 0.0629 0.021 Uiso 1 1 calc R . . C29 C 0.53281(14) 0.07140(7) 0.21528(10) 0.0166(4) Uani 1 1 d . . . H29 H 0.4807 0.0944 0.2224 0.020 Uiso 1 1 calc R . . C27 C 0.67789(14) 0.05161(7) 0.16276(10) 0.0171(4) Uani 1 1 d . . . H27 H 0.7251 0.0606 0.1332 0.021 Uiso 1 1 calc R . . C47 C 0.23984(14) 0.03221(7) -0.04187(10) 0.0170(4) Uani 1 1 d . . . H47 H 0.2057 0.0457 -0.0847 0.020 Uiso 1 1 calc R . . C46 C 0.33859(14) 0.04661(7) -0.01690(10) 0.0182(4) Uani 1 1 d . . . H46 H 0.3724 0.0697 -0.0429 0.022 Uiso 1 1 calc R . . C28 C 0.60236(13) 0.08533(7) 0.17292(10) 0.0155(4) Uani 1 1 d . . . H28 H 0.5982 0.1177 0.1511 0.019 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 I4 0.00771(5) 0.01060(5) 0.01042(5) 0.00093(4) -0.00037(4) 0.00056(4) I3 0.00615(5) 0.01160(5) 0.01429(6) 0.00065(4) 0.00021(4) -0.00092(4) I2 0.00820(5) 0.01095(5) 0.01063(5) 0.00025(4) 0.00143(4) 0.00082(4) I1 0.01018(6) 0.00887(5) 0.01476(6) -0.00141(4) 0.00295(4) 0.00065(4) Cu1 0.00901(10) 0.01025(10) 0.01320(11) -0.00116(8) 0.00052(8) 0.00002(8) Cu4 0.01044(11) 0.01163(10) 0.01457(11) -0.00073(9) 0.00284(9) -0.00024(8) Cu2 0.00783(10) 0.01094(10) 0.01330(11) -0.00047(8) 0.00047(8) -0.00092(8) Cu3 0.00804(10) 0.01217(10) 0.01412(11) 0.00149(9) 0.00031(8) 0.00140(8) P1 0.0065(2) 0.0098(2) 0.0122(2) -0.00043(17) 0.00104(17) -0.00051(16) P4 0.0093(2) 0.0101(2) 0.0159(2) -0.00146(18) 0.00437(18) -0.00067(17) P2 0.0082(2) 0.0101(2) 0.0105(2) -0.00046(17) 0.00057(17) -0.00060(17) P3 0.0075(2) 0.0109(2) 0.0122(2) 0.00048(17) 0.00015(17) 0.00084(17) C10 0.0101(9) 0.0168(9) 0.0228(10) 0.0067(8) 0.0023(8) -0.0026(7) C58 0.0218(11) 0.0139(9) 0.0309(12) -0.0001(8) 0.0110(9) -0.0051(8) C9 0.0151(10) 0.0138(9) 0.0240(11) -0.0010(8) 0.0020(8) -0.0042(7) C57 0.0176(10) 0.0175(9) 0.0229(11) 0.0068(8) 0.0060(8) 0.0011(8) C11 0.0139(9) 0.0206(10) 0.0156(10) 0.0032(8) 0.0040(7) 0.0012(8) C59 0.0228(11) 0.0176(9) 0.0240(11) -0.0064(8) 0.0077(8) -0.0071(8) C8 0.0141(9) 0.0164(9) 0.0176(10) -0.0021(7) 0.0054(7) -0.0021(7) C56 0.0122(9) 0.0163(9) 0.0210(10) 0.0002(8) 0.0029(7) 0.0005(7) C12 0.0098(9) 0.0138(8) 0.0157(9) -0.0006(7) 0.0004(7) 0.0006(7) C5 0.0146(10) 0.0172(10) 0.0499(15) 0.0127(10) 0.0049(9) 0.0047(8) C7 0.0071(8) 0.0119(8) 0.0135(9) 0.0014(7) 0.0003(7) -0.0001(7) C60 0.0222(10) 0.0162(9) 0.0177(10) -0.0023(8) 0.0095(8) -0.0043(8) C6 0.0109(9) 0.0157(9) 0.0341(12) 0.0070(8) 0.0031(8) -0.0012(7) C55 0.0112(9) 0.0101(8) 0.0197(10) -0.0019(7) 0.0071(7) 0.0013(7) C69 0.0124(10) 0.0385(13) 0.0240(11) 0.0074(10) 0.0036(8) 0.0028(9) C68 0.0137(10) 0.0213(10) 0.0218(11) -0.0008(8) 0.0056(8) 0.0014(8) C4 0.0085(9) 0.0241(11) 0.0380(13) 0.0100(9) 0.0034(9) 0.0043(8) C70 0.0134(10) 0.0511(15) 0.0181(11) -0.0023(10) 0.0029(8) -0.0044(10) C1 0.0112(9) 0.0130(8) 0.0138(9) 0.0009(7) 0.0020(7) 0.0014(7) C67 0.0101(9) 0.0179(9) 0.0136(9) -0.0004(7) 0.0054(7) -0.0022(7) C66 0.0299(12) 0.0161(10) 0.0333(13) 0.0069(9) 0.0191(10) 0.0055(9) C13 0.0112(9) 0.0099(8) 0.0132(9) -0.0007(7) 0.0014(7) 0.0005(7) C18 0.0125(9) 0.0295(11) 0.0173(10) 0.0011(8) 0.0030(7) 0.0003(8) C3 0.0096(9) 0.0180(9) 0.0257(11) 0.0040(8) 0.0006(8) -0.0036(7) C71 0.0219(11) 0.0366(12) 0.0240(12) -0.0123(10) 0.0051(9) -0.0079(10) C65 0.0323(13) 0.0213(11) 0.0442(15) 0.0042(10) 0.0282(11) 0.0043(9) C17 0.0147(10) 0.0293(11) 0.0195(10) -0.0013(9) -0.0042(8) 0.0011(8) C14 0.0150(10) 0.0239(10) 0.0172(10) -0.0030(8) 0.0049(8) -0.0046(8) C2 0.0109(9) 0.0130(8) 0.0198(10) 0.0015(7) 0.0002(7) -0.0001(7) C72 0.0175(10) 0.0224(10) 0.0209(11) -0.0055(8) 0.0047(8) -0.0025(8) C61 0.0096(9) 0.0103(8) 0.0240(10) -0.0044(7) 0.0064(7) -0.0025(7) C15 0.0278(12) 0.0343(12) 0.0153(10) -0.0014(9) 0.0082(9) -0.0082(10) C16 0.0277(11) 0.0215(10) 0.0121(10) -0.0026(8) -0.0015(8) -0.0014(8) C64 0.0115(10) 0.0191(10) 0.0401(13) -0.0080(9) 0.0093(9) 0.0001(8) C62 0.0111(9) 0.0232(10) 0.0177(10) -0.0056(8) -0.0003(7) 0.0008(8) C63 0.0145(10) 0.0221(10) 0.0261(11) -0.0057(9) -0.0051(8) 0.0040(8) C33 0.0099(9) 0.0117(9) 0.0362(12) 0.0021(8) -0.0022(8) -0.0001(7) C23 0.0430(14) 0.0328(12) 0.0145(11) -0.0010(9) 0.0063(9) -0.0119(11) C52 0.0313(12) 0.0139(9) 0.0201(11) -0.0003(8) -0.0080(9) -0.0018(8) C34 0.0095(9) 0.0129(9) 0.0413(13) -0.0018(9) 0.0077(9) -0.0007(7) C24 0.0289(12) 0.0216(10) 0.0154(10) -0.0020(8) 0.0032(8) -0.0094(9) C51 0.0182(10) 0.0218(10) 0.0216(11) 0.0029(8) -0.0052(8) -0.0071(8) C53 0.0330(13) 0.0178(10) 0.0242(11) -0.0074(9) -0.0049(9) 0.0092(9) C32 0.0117(9) 0.0137(8) 0.0204(10) 0.0012(7) -0.0003(7) -0.0023(7) C35 0.0171(10) 0.0156(9) 0.0259(11) -0.0039(8) 0.0106(8) -0.0037(8) C54 0.0182(10) 0.0222(10) 0.0236(11) -0.0056(9) -0.0032(8) 0.0065(8) C22 0.0337(12) 0.0222(10) 0.0137(10) -0.0059(8) -0.0032(9) 0.0007(9) C31 0.0064(8) 0.0095(8) 0.0188(9) 0.0014(7) 0.0025(7) -0.0022(6) C50 0.0130(9) 0.0171(9) 0.0185(10) 0.0001(8) 0.0002(7) 0.0001(7) C36 0.0109(9) 0.0130(8) 0.0180(10) 0.0001(7) 0.0031(7) -0.0010(7) C49 0.0152(9) 0.0096(8) 0.0142(9) 0.0014(7) -0.0020(7) 0.0001(7) C19 0.0114(9) 0.0113(8) 0.0124(9) -0.0007(7) -0.0007(7) 0.0000(7) C42 0.0131(9) 0.0142(9) 0.0184(10) 0.0020(7) 0.0017(7) -0.0007(7) C41 0.0103(9) 0.0230(10) 0.0178(10) 0.0015(8) 0.0043(7) -0.0006(8) C21 0.0197(10) 0.0130(9) 0.0212(10) -0.0032(8) -0.0056(8) 0.0004(8) C20 0.0139(9) 0.0139(9) 0.0164(10) 0.0014(7) -0.0015(7) -0.0002(7) C37 0.0057(8) 0.0128(8) 0.0121(9) -0.0012(7) -0.0013(6) 0.0000(6) C40 0.0103(9) 0.0190(9) 0.0207(10) -0.0052(8) 0.0041(7) 0.0016(7) C25 0.0099(8) 0.0112(8) 0.0101(8) -0.0005(7) -0.0020(6) -0.0003(7) C43 0.0098(8) 0.0114(8) 0.0123(9) -0.0017(7) 0.0036(7) 0.0013(7) C38 0.0123(9) 0.0133(8) 0.0137(9) 0.0003(7) 0.0027(7) -0.0004(7) C39 0.0137(9) 0.0117(8) 0.0219(10) -0.0013(7) 0.0021(8) 0.0019(7) C30 0.0104(9) 0.0141(9) 0.0192(10) 0.0002(7) 0.0036(7) -0.0014(7) C44 0.0145(9) 0.0125(8) 0.0141(9) -0.0002(7) 0.0003(7) -0.0006(7) C26 0.0124(9) 0.0137(8) 0.0185(10) 0.0015(7) 0.0049(7) 0.0018(7) C48 0.0105(9) 0.0197(9) 0.0147(9) -0.0013(7) 0.0012(7) -0.0001(7) C45 0.0148(10) 0.0180(9) 0.0196(10) -0.0012(8) 0.0023(8) -0.0036(8) C29 0.0129(9) 0.0136(9) 0.0230(10) 0.0008(7) 0.0024(8) 0.0028(7) C27 0.0155(10) 0.0167(9) 0.0203(10) 0.0039(8) 0.0064(8) -0.0004(7) C47 0.0184(10) 0.0216(10) 0.0109(9) 0.0016(7) 0.0020(7) 0.0024(8) C46 0.0204(10) 0.0184(9) 0.0168(10) 0.0019(8) 0.0059(8) -0.0030(8) C28 0.0162(10) 0.0124(8) 0.0167(10) 0.0031(7) -0.0007(7) -0.0009(7) _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 I4 Cu1 2.6387(3) . ? I4 Cu2 2.6819(3) . ? I4 Cu4 2.6922(2) . ? I4 I1 4.23725(17) . ? I4 I2 4.4105(3) . ? I4 I3 4.4821(3) . ? I3 Cu1 2.6538(2) . ? I3 Cu3 2.6783(2) . ? I3 Cu4 2.6907(3) . ? I3 I1 4.3172(2) . ? I3 I2 4.3507(2) . ? I2 Cu3 2.6681(3) . ? I2 Cu2 2.6759(3) . ? I2 Cu1 2.6989(3) . ? I2 I1 4.5147(3) . ? I1 Cu3 2.6591(3) . ? I1 Cu2 2.6787(3) . ? I1 Cu4 2.7033(2) . ? Cu1 P1 2.2520(5) . ? Cu1 Cu2 2.7872(3) . ? Cu1 Cu4 2.7944(3) . ? Cu1 Cu3 2.7977(3) . ? Cu4 P4 2.2598(5) . ? Cu4 Cu3 2.9833(4) . ? Cu4 Cu2 3.0650(3) . ? Cu2 P2 2.2527(5) . ? Cu2 Cu3 2.7368(3) . ? Cu3 P3 2.2499(5) . ? P1 C13 1.8148(18) . ? P1 C7 1.8218(17) . ? P1 C1 1.8307(18) . ? P4 C67 1.8237(19) . ? P4 C55 1.8319(18) . ? P4 C61 1.8345(18) . ? P2 C19 1.8189(18) . ? P2 C31 1.8248(17) . ? P2 C25 1.8295(18) . ? P3 C43 1.8182(18) . ? P3 C37 1.8213(17) . ? P3 C49 1.8238(18) . ? C10 C11 1.383(3) . ? C10 C9 1.387(3) . ? C58 C59 1.380(3) . ? C58 C57 1.385(3) . ? C9 C8 1.383(2) . ? C57 C56 1.387(2) . ? C11 C12 1.390(2) . ? C59 C60 1.393(2) . ? C8 C7 1.398(2) . ? C56 C55 1.392(3) . ? C12 C7 1.392(2) . ? C5 C4 1.385(3) . ? C5 C6 1.393(3) . ? C60 C55 1.394(3) . ? C6 C1 1.389(2) . ? C69 C70 1.376(3) . ? C69 C68 1.387(3) . ? C68 C67 1.397(2) . ? C4 C3 1.383(3) . ? C70 C71 1.384(3) . ? C1 C2 1.397(2) . ? C67 C72 1.386(3) . ? C66 C65 1.390(3) . ? C66 C61 1.395(3) . ? C13 C14 1.388(2) . ? C13 C18 1.390(2) . ? C18 C17 1.382(3) . ? C3 C2 1.389(2) . ? C71 C72 1.391(3) . ? C65 C64 1.376(3) . ? C17 C16 1.385(3) . ? C14 C15 1.388(3) . ? C61 C62 1.381(3) . ? C15 C16 1.380(3) . ? C64 C63 1.375(3) . ? C62 C63 1.397(3) . ? C33 C34 1.380(3) . ? C33 C32 1.388(3) . ? C23 C22 1.381(3) . ? C23 C24 1.387(3) . ? C52 C51 1.380(3) . ? C52 C53 1.382(3) . ? C34 C35 1.392(3) . ? C24 C19 1.391(3) . ? C51 C50 1.389(3) . ? C53 C54 1.388(3) . ? C32 C31 1.397(2) . ? C35 C36 1.392(2) . ? C54 C49 1.400(3) . ? C22 C21 1.378(3) . ? C31 C36 1.397(2) . ? C50 C49 1.391(2) . ? C19 C20 1.397(2) . ? C42 C41 1.383(2) . ? C42 C37 1.398(2) . ? C41 C40 1.392(3) . ? C21 C20 1.380(3) . ? C37 C38 1.389(2) . ? C40 C39 1.380(3) . ? C25 C26 1.391(2) . ? C25 C30 1.395(2) . ? C43 C48 1.391(2) . ? C43 C44 1.399(2) . ? C38 C39 1.391(2) . ? C30 C29 1.386(2) . ? C44 C45 1.387(2) . ? C26 C27 1.393(2) . ? C48 C47 1.385(2) . ? C45 C46 1.385(3) . ? C29 C28 1.387(2) . ? C27 C28 1.384(2) . ? C47 C46 1.385(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I4 Cu2 63.177(7) . . ? Cu1 I4 Cu4 63.218(9) . . ? Cu2 I4 Cu4 69.545(8) . . ? Cu1 I4 I1 73.219(6) . . ? Cu2 I4 I1 37.747(6) . . ? Cu4 I4 I1 38.341(5) . . ? Cu1 I4 I2 34.720(6) . . ? Cu2 I4 I2 34.551(5) . . ? Cu4 I4 I2 76.925(8) . . ? I1 I4 I2 62.904(4) . . ? Cu1 I4 I3 32.228(6) . . ? Cu2 I4 I3 71.557(6) . . ? Cu4 I4 I3 33.617(6) . . ? I1 I4 I3 59.277(3) . . ? I2 I4 I3 58.575(6) . . ? Cu1 I3 Cu3 63.293(7) . . ? Cu1 I3 Cu4 63.043(9) . . ? Cu3 I3 Cu4 67.510(8) . . ? Cu1 I3 I1 71.634(6) . . ? Cu3 I3 I1 35.866(6) . . ? Cu4 I3 I1 36.935(5) . . ? Cu1 I3 I2 35.976(5) . . ? Cu3 I3 I2 35.457(5) . . ? Cu4 I3 I2 78.070(7) . . ? I1 I3 I2 62.778(4) . . ? Cu1 I3 I4 32.023(6) . . ? Cu3 I3 I4 70.402(6) . . ? Cu4 I3 I4 33.638(6) . . ? I1 I3 I4 57.536(3) . . ? I2 I3 I4 59.890(4) . . ? Cu3 I2 Cu2 61.610(9) . . ? Cu3 I2 Cu1 62.833(8) . . ? Cu2 I2 Cu1 62.472(8) . . ? Cu3 I2 I3 35.613(5) . . ? Cu2 I2 I3 74.013(8) . . ? Cu1 I2 I3 35.284(6) . . ? Cu3 I2 I4 71.772(7) . . ? Cu2 I2 I4 34.638(6) . . ? Cu1 I2 I4 33.840(5) . . ? I3 I2 I4 61.535(6) . . ? Cu3 I2 I1 32.001(6) . . ? Cu2 I2 I1 32.547(5) . . ? Cu1 I2 I1 67.806(6) . . ? I3 I2 I1 58.248(5) . . ? I4 I2 I1 56.672(4) . . ? Cu3 I1 Cu2 61.689(8) . . ? Cu3 I1 Cu4 67.600(8) . . ? Cu2 I1 Cu4 69.427(7) . . ? Cu3 I1 I4 75.044(7) . . ? Cu2 I1 I4 37.800(5) . . ? Cu4 I1 I4 38.155(5) . . ? Cu3 I1 I3 36.166(6) . . ? Cu2 I1 I3 74.612(6) . . ? Cu4 I1 I3 36.735(6) . . ? I4 I1 I3 63.187(4) . . ? Cu3 I1 I2 32.122(5) . . ? Cu2 I1 I2 32.509(6) . . ? Cu4 I1 I2 74.893(6) . . ? I4 I1 I2 60.425(4) . . ? I3 I1 I2 58.974(4) . . ? P1 Cu1 I4 105.866(15) . . ? P1 Cu1 I3 107.758(14) . . ? I4 Cu1 I3 115.748(10) . . ? P1 Cu1 I2 106.832(15) . . ? I4 Cu1 I2 111.440(9) . . ? I3 Cu1 I2 108.739(9) . . ? P1 Cu1 Cu2 142.963(15) . . ? I4 Cu1 Cu2 59.168(7) . . ? I3 Cu1 Cu2 109.199(9) . . ? I2 Cu1 Cu2 58.362(8) . . ? P1 Cu1 Cu4 138.747(15) . . ? I4 Cu1 Cu4 59.325(8) . . ? I3 Cu1 Cu4 59.124(8) . . ? I2 Cu1 Cu4 114.420(10) . . ? Cu2 Cu1 Cu4 66.612(8) . . ? P1 Cu1 Cu3 146.630(16) . . ? I4 Cu1 Cu3 107.419(9) . . ? I3 Cu1 Cu3 58.781(7) . . ? I2 Cu1 Cu3 58.045(7) . . ? Cu2 Cu1 Cu3 58.685(8) . . ? Cu4 Cu1 Cu3 64.482(8) . . ? P4 Cu4 I3 116.874(15) . . ? P4 Cu4 I4 106.576(16) . . ? I3 Cu4 I4 112.745(10) . . ? P4 Cu4 I1 110.013(14) . . ? I3 Cu4 I1 106.330(9) . . ? I4 Cu4 I1 103.504(8) . . ? P4 Cu4 Cu1 146.422(16) . . ? I3 Cu4 Cu1 57.832(7) . . ? I4 Cu4 Cu1 57.457(8) . . ? I1 Cu4 Cu1 102.790(9) . . ? P4 Cu4 Cu3 151.548(16) . . ? I3 Cu4 Cu3 56.046(8) . . ? I4 Cu4 Cu3 100.989(10) . . ? I1 Cu4 Cu3 55.495(7) . . ? Cu1 Cu4 Cu3 57.812(8) . . ? P4 Cu4 Cu2 142.495(16) . . ? I3 Cu4 Cu2 100.628(10) . . ? I4 Cu4 Cu2 55.070(6) . . ? I1 Cu4 Cu2 54.909(6) . . ? Cu1 Cu4 Cu2 56.582(8) . . ? Cu3 Cu4 Cu2 53.787(8) . . ? P2 Cu2 I2 108.025(15) . . ? P2 Cu2 I1 107.347(14) . . ? I2 Cu2 I1 114.944(10) . . ? P2 Cu2 I4 111.226(15) . . ? I2 Cu2 I4 110.811(9) . . ? I1 Cu2 I4 104.453(9) . . ? P2 Cu2 Cu3 140.694(15) . . ? I2 Cu2 Cu3 59.053(9) . . ? I1 Cu2 Cu3 58.803(7) . . ? I4 Cu2 Cu3 107.962(9) . . ? P2 Cu2 Cu1 148.955(15) . . ? I2 Cu2 Cu1 59.167(7) . . ? I1 Cu2 Cu1 103.621(9) . . ? I4 Cu2 Cu1 57.655(8) . . ? Cu3 Cu2 Cu1 60.848(8) . . ? P2 Cu2 Cu4 145.048(16) . . ? I2 Cu2 Cu4 106.919(10) . . ? I1 Cu2 Cu4 55.664(7) . . ? I4 Cu2 Cu4 55.385(7) . . ? Cu3 Cu2 Cu4 61.581(8) . . ? Cu1 Cu2 Cu4 56.806(8) . . ? P3 Cu3 I1 110.442(15) . . ? P3 Cu3 I2 107.378(15) . . ? I1 Cu3 I2 115.877(9) . . ? P3 Cu3 I3 105.782(14) . . ? I1 Cu3 I3 107.968(9) . . ? I2 Cu3 I3 108.930(8) . . ? P3 Cu3 Cu2 144.192(16) . . ? I1 Cu3 Cu2 59.508(8) . . ? I2 Cu3 Cu2 59.336(8) . . ? I3 Cu3 Cu2 109.995(9) . . ? P3 Cu3 Cu1 145.424(16) . . ? I1 Cu3 Cu1 103.856(10) . . ? I2 Cu3 Cu1 59.121(7) . . ? I3 Cu3 Cu1 57.926(7) . . ? Cu2 Cu3 Cu1 60.467(8) . . ? P3 Cu3 Cu4 142.702(16) . . ? I1 Cu3 Cu4 56.905(7) . . ? I2 Cu3 Cu4 109.484(10) . . ? I3 Cu3 Cu4 56.444(7) . . ? Cu2 Cu3 Cu4 64.632(9) . . ? Cu1 Cu3 Cu4 57.706(8) . . ? C13 P1 C7 103.26(8) . . ? C13 P1 C1 105.70(8) . . ? C7 P1 C1 105.22(8) . . ? C13 P1 Cu1 110.75(6) . . ? C7 P1 Cu1 117.10(6) . . ? C1 P1 Cu1 113.72(6) . . ? C67 P4 C55 104.14(8) . . ? C67 P4 C61 104.11(8) . . ? C55 P4 C61 101.28(8) . . ? C67 P4 Cu4 112.88(6) . . ? C55 P4 Cu4 116.58(6) . . ? C61 P4 Cu4 116.19(6) . . ? C19 P2 C31 104.25(8) . . ? C19 P2 C25 101.17(8) . . ? C31 P2 C25 105.45(8) . . ? C19 P2 Cu2 116.65(6) . . ? C31 P2 Cu2 112.86(6) . . ? C25 P2 Cu2 115.02(6) . . ? C43 P3 C37 104.65(8) . . ? C43 P3 C49 103.51(8) . . ? C37 P3 C49 103.80(8) . . ? C43 P3 Cu3 115.62(6) . . ? C37 P3 Cu3 114.35(6) . . ? C49 P3 Cu3 113.57(6) . . ? C11 C10 C9 119.81(17) . . ? C59 C58 C57 119.95(18) . . ? C8 C9 C10 120.16(18) . . ? C58 C57 C56 120.33(18) . . ? C10 C11 C12 120.22(18) . . ? C58 C59 C60 119.93(19) . . ? C9 C8 C7 120.62(17) . . ? C57 C56 C55 120.36(18) . . ? C11 C12 C7 120.45(17) . . ? C4 C5 C6 120.21(18) . . ? C12 C7 C8 118.73(16) . . ? C12 C7 P1 118.69(13) . . ? C8 C7 P1 122.57(14) . . ? C59 C60 C55 120.55(18) . . ? C1 C6 C5 120.57(17) . . ? C56 C55 C60 118.88(17) . . ? C56 C55 P4 123.81(14) . . ? C60 C55 P4 117.16(14) . . ? C70 C69 C68 120.4(2) . . ? C69 C68 C67 120.49(19) . . ? C3 C4 C5 119.66(18) . . ? C69 C70 C71 119.7(2) . . ? C6 C1 C2 118.68(16) . . ? C6 C1 P1 123.79(14) . . ? C2 C1 P1 117.52(13) . . ? C72 C67 C68 118.62(18) . . ? C72 C67 P4 120.90(15) . . ? C68 C67 P4 120.24(14) . . ? C65 C66 C61 119.81(19) . . ? C14 C13 C18 118.43(17) . . ? C14 C13 P1 122.37(14) . . ? C18 C13 P1 118.63(14) . . ? C17 C18 C13 121.32(18) . . ? C4 C3 C2 120.25(17) . . ? C70 C71 C72 120.2(2) . . ? C64 C65 C66 120.6(2) . . ? C18 C17 C16 119.80(18) . . ? C15 C14 C13 120.21(18) . . ? C3 C2 C1 120.57(17) . . ? C67 C72 C71 120.59(19) . . ? C62 C61 C66 119.23(17) . . ? C62 C61 P4 119.42(14) . . ? C66 C61 P4 121.28(15) . . ? C16 C15 C14 120.85(19) . . ? C15 C16 C17 119.37(19) . . ? C63 C64 C65 119.84(19) . . ? C61 C62 C63 120.36(19) . . ? C64 C63 C62 120.11(19) . . ? C34 C33 C32 120.83(18) . . ? C22 C23 C24 120.1(2) . . ? C51 C52 C53 119.87(19) . . ? C33 C34 C35 119.69(18) . . ? C23 C24 C19 120.35(19) . . ? C52 C51 C50 120.33(19) . . ? C52 C53 C54 120.27(19) . . ? C33 C32 C31 120.22(18) . . ? C36 C35 C34 119.73(19) . . ? C53 C54 C49 120.28(19) . . ? C21 C22 C23 120.08(19) . . ? C32 C31 C36 118.68(16) . . ? C32 C31 P2 122.19(14) . . ? C36 C31 P2 118.90(13) . . ? C51 C50 C49 120.45(18) . . ? C35 C36 C31 120.79(17) . . ? C50 C49 C54 118.79(17) . . ? C50 C49 P3 123.53(14) . . ? C54 C49 P3 117.63(14) . . ? C24 C19 C20 118.81(17) . . ? C24 C19 P2 119.73(14) . . ? C20 C19 P2 121.46(14) . . ? C41 C42 C37 120.31(17) . . ? C42 C41 C40 120.05(18) . . ? C22 C21 C20 120.21(18) . . ? C21 C20 C19 120.48(18) . . ? C38 C37 C42 119.18(16) . . ? C38 C37 P3 123.93(14) . . ? C42 C37 P3 116.89(13) . . ? C39 C40 C41 119.93(17) . . ? C26 C25 C30 118.30(16) . . ? C26 C25 P2 124.30(13) . . ? C30 C25 P2 117.39(13) . . ? C48 C43 C44 119.11(16) . . ? C48 C43 P3 122.52(14) . . ? C44 C43 P3 118.37(13) . . ? C37 C38 C39 120.32(17) . . ? C40 C39 C38 120.18(17) . . ? C29 C30 C25 120.80(17) . . ? C45 C44 C43 120.18(17) . . ? C25 C26 C27 120.92(17) . . ? C47 C48 C43 120.44(17) . . ? C46 C45 C44 120.10(18) . . ? C30 C29 C28 120.40(17) . . ? C28 C27 C26 120.15(17) . . ? C46 C47 C48 120.14(18) . . ? C47 C46 C45 120.02(18) . . ? C27 C28 C29 119.43(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.781 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.088 data_cuipph_mono_020k _database_code_depnum_ccdc_archive 'CCDC 777574' #TrackingRef 'mono-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method chloroform/ether _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 11(1) _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 0.0007 0.0011 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' H H 0.0000 0.0000 'International Tables Vol C Tables 6.1.1.4' Cu Cu 0.2733 0.9097 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' I I -1.0407 1.3054 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' P P 0.0618 0.0648 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 13.3862(2) _cell_length_b 26.2858(5) _cell_length_c 19.3801(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.410(7) _cell_angle_gamma 90.00 _cell_volume 6727.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 20(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 1.85 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8399 _exptl_absorpt_correction_T_max 0.9478 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.5886 _diffrn_source 'SPring-8 BL02B1 bending magnet' _diffrn_source_type 'SPring-8 beamline BL02B1' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'SPring-8 BL02B1 Large cylindrical Image-Plate camera' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 109078 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 24.49 _reflns_number_total 19657 _reflns_number_gt 15999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_cell_refinement 'R-AXIS (Rigaku Co. Ltd., 2008)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2008), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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. Anomalous dispersion parameters are taken from S. Sasaki, KEK Report 88-14, 1-136 (1989). ; _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^)+(0.0151P)^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 19657 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0381 _refine_ls_wR_factor_gt 0.0379 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _refine_ls_shift/su_max 0.002 _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 I4 I 0.491555(8) -0.201559(4) 0.341022(6) 0.00630(2) Uani 1 1 d . . . I3 I 0.182185(8) -0.196544(4) 0.210800(6) 0.00686(2) Uani 1 1 d . . . I2 I 0.442579(8) -0.139302(4) 0.126555(6) 0.00643(2) Uani 1 1 d . . . I1 I 0.330759(8) -0.062403(4) 0.308088(6) 0.00709(2) Uani 1 1 d . . . Cu1 Cu 0.380558(16) -0.206800(8) 0.215523(11) 0.00736(4) Uani 1 1 d . . . Cu4 Cu 0.302765(16) -0.163025(8) 0.326672(12) 0.00802(4) Uani 1 1 d . . . Cu2 Cu 0.476692(16) -0.116765(8) 0.263088(12) 0.00732(4) Uani 1 1 d . . . Cu3 Cu 0.285688(16) -0.112711(8) 0.187930(12) 0.00779(4) Uani 1 1 d . . . P1 P 0.40796(3) -0.284968(17) 0.17465(2) 0.00654(8) Uani 1 1 d . . . P4 P 0.24842(3) -0.176083(17) 0.42982(2) 0.00751(9) Uani 1 1 d . . . P2 P 0.61992(3) -0.070399(17) 0.28513(2) 0.00663(8) Uani 1 1 d . . . P3 P 0.17985(3) -0.066374(17) 0.11014(2) 0.00684(8) Uani 1 1 d . . . C10 C 0.24360(14) -0.41740(7) 0.26527(10) 0.0119(4) Uani 1 1 d . . . H10 H 0.2100 -0.4445 0.2845 0.014 Uiso 1 1 calc R . . C58 C 0.08187(14) -0.32784(7) 0.45150(10) 0.0141(4) Uani 1 1 d . . . H58 H 0.0447 -0.3582 0.4552 0.017 Uiso 1 1 calc R . . C9 C 0.27710(14) -0.42374(7) 0.20170(10) 0.0124(4) Uani 1 1 d . . . H9 H 0.2664 -0.4552 0.1775 0.015 Uiso 1 1 calc R . . C57 C 0.13898(14) -0.30651(7) 0.51068(10) 0.0128(4) Uani 1 1 d . . . H57 H 0.1413 -0.3226 0.5548 0.015 Uiso 1 1 calc R . . C11 C 0.25924(14) -0.37147(7) 0.30062(10) 0.0122(4) Uani 1 1 d . . . H11 H 0.2362 -0.3671 0.3441 0.015 Uiso 1 1 calc R . . C59 C 0.07922(14) -0.30461(7) 0.38705(10) 0.0137(4) Uani 1 1 d . . . H59 H 0.0407 -0.3193 0.3464 0.016 Uiso 1 1 calc R . . C8 C 0.32594(13) -0.38440(7) 0.17345(10) 0.0108(4) Uani 1 1 d . . . H8 H 0.3477 -0.3889 0.1296 0.013 Uiso 1 1 calc R . . C56 C 0.19292(13) -0.26168(7) 0.50577(10) 0.0110(4) Uani 1 1 d . . . H56 H 0.2319 -0.2473 0.5465 0.013 Uiso 1 1 calc R . . C12 C 0.30868(13) -0.33181(7) 0.27250(9) 0.0095(3) Uani 1 1 d . . . H12 H 0.3187 -0.3003 0.2967 0.011 Uiso 1 1 calc R . . C5 C 0.67865(14) -0.36404(7) 0.20639(11) 0.0169(4) Uani 1 1 d . . . H5 H 0.7012 -0.3982 0.2140 0.020 Uiso 1 1 calc R . . C7 C 0.34352(13) -0.33802(7) 0.20905(9) 0.0081(3) Uani 1 1 d . . . C60 C 0.13297(14) -0.25987(7) 0.38184(10) 0.0119(4) Uani 1 1 d . . . H60 H 0.1310 -0.2442 0.3375 0.014 Uiso 1 1 calc R . . C6 C 0.57595(14) -0.35290(7) 0.19879(10) 0.0133(4) Uani 1 1 d . . . H6 H 0.5287 -0.3795 0.2017 0.016 Uiso 1 1 calc R . . C55 C 0.18963(13) -0.23784(6) 0.44107(10) 0.0086(3) Uani 1 1 d . . . C69 C 0.49486(14) -0.20841(8) 0.57859(10) 0.0163(4) Uani 1 1 d . . . H69 H 0.5377 -0.2368 0.5915 0.020 Uiso 1 1 calc R . . C68 C 0.41461(14) -0.21251(7) 0.52359(10) 0.0125(4) Uani 1 1 d . . . H68 H 0.4037 -0.2436 0.4984 0.015 Uiso 1 1 calc R . . C4 C 0.74835(14) -0.32538(7) 0.20293(10) 0.0148(4) Uani 1 1 d . . . H4 H 0.8184 -0.3331 0.2074 0.018 Uiso 1 1 calc R . . C70 C 0.51240(14) -0.16300(8) 0.61455(10) 0.0176(4) Uani 1 1 d . . . H70 H 0.5670 -0.1603 0.6524 0.021 Uiso 1 1 calc R . . C1 C 0.54181(13) -0.30325(7) 0.18696(9) 0.0085(3) Uani 1 1 d . . . C67 C 0.34948(13) -0.17121(7) 0.50481(9) 0.0094(3) Uani 1 1 d . . . C66 C 0.11407(15) -0.13588(7) 0.51403(11) 0.0151(4) Uani 1 1 d . . . H66 H 0.1426 -0.1598 0.5485 0.018 Uiso 1 1 calc R . . C13 C 0.36347(13) -0.28844(6) 0.08104(9) 0.0080(3) Uani 1 1 d . . . C18 C 0.26088(14) -0.29730(7) 0.05752(10) 0.0132(4) Uani 1 1 d . . . H18 H 0.2177 -0.3053 0.0903 0.016 Uiso 1 1 calc R . . C3 C 0.71585(14) -0.27560(7) 0.19298(10) 0.0123(4) Uani 1 1 d . . . H3 H 0.7636 -0.2491 0.1914 0.015 Uiso 1 1 calc R . . C71 C 0.45043(15) -0.12139(8) 0.59545(11) 0.0171(4) Uani 1 1 d . . . H71 H 0.4631 -0.0901 0.6197 0.021 Uiso 1 1 calc R . . C65 C 0.03533(15) -0.10435(7) 0.52625(11) 0.0177(4) Uani 1 1 d . . . H65 H 0.0090 -0.1075 0.5687 0.021 Uiso 1 1 calc R . . C17 C 0.22119(15) -0.29459(7) -0.01297(10) 0.0146(4) Uani 1 1 d . . . H17 H 0.1513 -0.3010 -0.0283 0.018 Uiso 1 1 calc R . . C14 C 0.42517(14) -0.27570(7) 0.03232(10) 0.0118(4) Uani 1 1 d . . . H14 H 0.4950 -0.2689 0.0475 0.014 Uiso 1 1 calc R . . C2 C 0.61273(13) -0.26444(7) 0.18525(10) 0.0103(3) Uani 1 1 d . . . H2 H 0.5905 -0.2302 0.1788 0.012 Uiso 1 1 calc R . . C72 C 0.36955(14) -0.12559(7) 0.54063(10) 0.0134(4) Uani 1 1 d . . . H72 H 0.3275 -0.0969 0.5275 0.016 Uiso 1 1 calc R . . C61 C 0.15106(13) -0.13229(7) 0.45083(10) 0.0097(3) Uani 1 1 d . . . C15 C 0.38495(15) -0.27291(8) -0.03838(10) 0.0157(4) Uani 1 1 d . . . H15 H 0.4277 -0.2644 -0.0713 0.019 Uiso 1 1 calc R . . C16 C 0.28332(15) -0.28246(7) -0.06135(10) 0.0146(4) Uani 1 1 d . . . H16 H 0.2563 -0.2807 -0.1098 0.017 Uiso 1 1 calc R . . C64 C -0.00490(14) -0.06859(7) 0.47731(11) 0.0145(4) Uani 1 1 d . . . H64 H -0.0582 -0.0470 0.4863 0.017 Uiso 1 1 calc R . . C62 C 0.10963(14) -0.09651(7) 0.40162(10) 0.0117(4) Uani 1 1 d . . . H62 H 0.1340 -0.0940 0.3584 0.014 Uiso 1 1 calc R . . C63 C 0.03243(14) -0.06428(7) 0.41529(10) 0.0139(4) Uani 1 1 d . . . H63 H 0.0055 -0.0393 0.3819 0.017 Uiso 1 1 calc R . . C33 C 0.88684(14) -0.15009(7) 0.29679(11) 0.0133(4) Uani 1 1 d . . . H33 H 0.9392 -0.1620 0.3322 0.016 Uiso 1 1 calc R . . C23 C 0.64557(16) -0.05609(8) 0.49744(10) 0.0184(4) Uani 1 1 d . . . H23 H 0.6165 -0.0716 0.5338 0.022 Uiso 1 1 calc R . . C52 C -0.01125(15) -0.16745(7) -0.05642(10) 0.0153(4) Uani 1 1 d . . . H52 H -0.0494 -0.1884 -0.0910 0.018 Uiso 1 1 calc R . . C34 C 0.88981(14) -0.16150(7) 0.22734(11) 0.0142(4) Uani 1 1 d . . . H34 H 0.9444 -0.1807 0.2152 0.017 Uiso 1 1 calc R . . C24 C 0.61645(15) -0.07182(7) 0.42859(10) 0.0141(4) Uani 1 1 d . . . H24 H 0.5671 -0.0979 0.4180 0.017 Uiso 1 1 calc R . . C51 C -0.06021(15) -0.13483(7) -0.01668(10) 0.0142(4) Uani 1 1 d . . . H51 H -0.1321 -0.1338 -0.0236 0.017 Uiso 1 1 calc R . . C53 C 0.09380(15) -0.16934(7) -0.04549(11) 0.0168(4) Uani 1 1 d . . . H53 H 0.1274 -0.1919 -0.0724 0.020 Uiso 1 1 calc R . . C32 C 0.80795(13) -0.12136(7) 0.31504(10) 0.0110(4) Uani 1 1 d . . . H32 H 0.8071 -0.1134 0.3628 0.013 Uiso 1 1 calc R . . C35 C 0.81275(14) -0.14473(7) 0.17571(10) 0.0126(4) Uani 1 1 d . . . H35 H 0.8150 -0.1521 0.1280 0.015 Uiso 1 1 calc R . . C54 C 0.14995(15) -0.13843(7) 0.00460(10) 0.0144(4) Uani 1 1 d . . . H54 H 0.2218 -0.1401 0.0121 0.017 Uiso 1 1 calc R . . C22 C 0.71670(15) -0.01799(7) 0.51309(10) 0.0155(4) Uani 1 1 d . . . H22 H 0.7362 -0.0072 0.5602 0.019 Uiso 1 1 calc R . . C31 C 0.73012(13) -0.10420(6) 0.26364(10) 0.0080(3) Uani 1 1 d . . . C50 C -0.00458(14) -0.10369(7) 0.03320(10) 0.0113(4) Uani 1 1 d . . . H50 H -0.0386 -0.0814 0.0602 0.014 Uiso 1 1 calc R . . C36 C 0.73206(13) -0.11705(7) 0.19370(10) 0.0097(3) Uani 1 1 d . . . H36 H 0.6780 -0.1068 0.1584 0.012 Uiso 1 1 calc R . . C49 C 0.10097(14) -0.10490(7) 0.04406(9) 0.0094(3) Uani 1 1 d . . . C19 C 0.65939(13) -0.04952(7) 0.37504(9) 0.0086(3) Uani 1 1 d . . . C42 C 0.03823(13) -0.05291(7) 0.19679(9) 0.0106(4) Uani 1 1 d . . . H42 H 0.0534 -0.0874 0.2089 0.013 Uiso 1 1 calc R . . C41 C -0.03357(14) -0.02710(7) 0.22731(10) 0.0117(4) Uani 1 1 d . . . H41 H -0.0692 -0.0441 0.2591 0.014 Uiso 1 1 calc R . . C21 C 0.75987(14) 0.00461(7) 0.46019(10) 0.0125(4) Uani 1 1 d . . . H21 H 0.8088 0.0308 0.4711 0.015 Uiso 1 1 calc R . . C20 C 0.73141(13) -0.01110(7) 0.39169(10) 0.0104(3) Uani 1 1 d . . . H20 H 0.7611 0.0044 0.3556 0.013 Uiso 1 1 calc R . . C37 C 0.08850(13) -0.02852(7) 0.14835(9) 0.0078(3) Uani 1 1 d . . . C40 C -0.05333(13) 0.02409(7) 0.21121(10) 0.0111(4) Uani 1 1 d . . . H40 H -0.1019 0.0420 0.2325 0.013 Uiso 1 1 calc R . . C25 C 0.61620(13) -0.00981(7) 0.23827(9) 0.0083(3) Uani 1 1 d . . . C43 C 0.24023(13) -0.02133(6) 0.05869(9) 0.0079(3) Uani 1 1 d . . . C38 C 0.06812(13) 0.02235(7) 0.13243(9) 0.0091(3) Uani 1 1 d . . . H38 H 0.1022 0.0392 0.0997 0.011 Uiso 1 1 calc R . . C39 C -0.00230(13) 0.04865(7) 0.16440(10) 0.0113(4) Uani 1 1 d . . . H39 H -0.0153 0.0836 0.1540 0.014 Uiso 1 1 calc R . . C30 C 0.53939(13) 0.02435(7) 0.24724(10) 0.0104(4) Uani 1 1 d . . . H30 H 0.4910 0.0151 0.2758 0.012 Uiso 1 1 calc R . . C44 C 0.33936(13) -0.00630(7) 0.08388(10) 0.0101(3) Uani 1 1 d . . . H44 H 0.3731 -0.0191 0.1273 0.012 Uiso 1 1 calc R . . C26 C 0.68543(13) 0.00451(7) 0.19548(10) 0.0100(3) Uani 1 1 d . . . H26 H 0.7381 -0.0182 0.1887 0.012 Uiso 1 1 calc R . . C48 C 0.19083(14) -0.00160(7) -0.00450(10) 0.0104(3) Uani 1 1 d . . . H48 H 0.1233 -0.0117 -0.0220 0.012 Uiso 1 1 calc R . . C45 C 0.38915(14) 0.02735(7) 0.04572(10) 0.0125(4) Uani 1 1 d . . . H45 H 0.4571 0.0370 0.0627 0.015 Uiso 1 1 calc R . . C29 C 0.53294(14) 0.07169(7) 0.21503(10) 0.0114(4) Uani 1 1 d . . . H29 H 0.4807 0.0947 0.2220 0.014 Uiso 1 1 calc R . . C27 C 0.67842(14) 0.05174(7) 0.16246(10) 0.0127(4) Uani 1 1 d . . . H27 H 0.7256 0.0608 0.1329 0.015 Uiso 1 1 calc R . . C47 C 0.23973(14) 0.03264(7) -0.04200(10) 0.0116(4) Uani 1 1 d . . . H47 H 0.2053 0.0465 -0.0846 0.014 Uiso 1 1 calc R . . C46 C 0.33942(14) 0.04670(7) -0.01707(10) 0.0122(4) Uani 1 1 d . . . H46 H 0.3734 0.0696 -0.0432 0.015 Uiso 1 1 calc R . . C28 C 0.60283(14) 0.08553(7) 0.17264(10) 0.0113(4) Uani 1 1 d . . . H28 H 0.5987 0.1180 0.1508 0.014 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 I4 0.00442(5) 0.00733(5) 0.00687(5) 0.00055(4) 0.00008(4) 0.00035(4) I3 0.00353(5) 0.00788(5) 0.00896(5) 0.00037(4) 0.00044(4) -0.00051(4) I2 0.00471(5) 0.00760(5) 0.00705(5) 0.00012(4) 0.00117(4) 0.00052(4) I1 0.00586(5) 0.00635(5) 0.00930(5) -0.00073(4) 0.00202(4) 0.00038(4) Cu1 0.00566(10) 0.00741(10) 0.00885(10) -0.00077(8) 0.00074(8) 0.00010(8) Cu4 0.00645(11) 0.00838(10) 0.00948(10) -0.00036(8) 0.00203(8) 0.00002(8) Cu2 0.00486(10) 0.00786(10) 0.00903(11) -0.00034(8) 0.00050(8) -0.00053(8) Cu3 0.00523(10) 0.00859(10) 0.00933(11) 0.00091(8) 0.00054(8) 0.00073(8) P1 0.0041(2) 0.00729(19) 0.0083(2) -0.00027(16) 0.00093(16) -0.00027(16) P4 0.0057(2) 0.0075(2) 0.0098(2) -0.00066(17) 0.00240(17) -0.00033(16) P2 0.0045(2) 0.0077(2) 0.0076(2) -0.00015(16) 0.00054(16) -0.00033(16) P3 0.0042(2) 0.0078(2) 0.0084(2) 0.00021(16) 0.00052(16) 0.00040(16) C10 0.0069(9) 0.0128(8) 0.0159(9) 0.0044(7) 0.0017(7) -0.0018(7) C58 0.0122(10) 0.0103(8) 0.0208(10) 0.0002(7) 0.0062(8) -0.0021(7) C9 0.0097(9) 0.0112(8) 0.0161(9) -0.0016(7) 0.0014(7) -0.0030(7) C57 0.0100(9) 0.0130(9) 0.0163(9) 0.0042(7) 0.0048(7) 0.0009(7) C11 0.0096(9) 0.0156(9) 0.0120(9) 0.0034(7) 0.0033(7) 0.0017(7) C59 0.0125(9) 0.0138(9) 0.0151(9) -0.0040(7) 0.0033(7) -0.0023(7) C8 0.0075(9) 0.0134(9) 0.0118(9) -0.0011(7) 0.0027(7) -0.0002(7) C56 0.0070(9) 0.0124(8) 0.0135(9) 0.0000(7) 0.0016(7) 0.0004(7) C12 0.0074(8) 0.0106(8) 0.0100(8) -0.0006(7) -0.0003(7) 0.0006(7) C5 0.0119(10) 0.0125(9) 0.0264(11) 0.0064(8) 0.0032(8) 0.0025(7) C7 0.0060(8) 0.0095(8) 0.0090(8) 0.0018(6) 0.0016(6) 0.0006(6) C60 0.0122(9) 0.0126(8) 0.0122(9) -0.0009(7) 0.0057(7) -0.0012(7) C6 0.0097(9) 0.0110(9) 0.0194(10) 0.0031(7) 0.0031(7) 0.0001(7) C55 0.0056(8) 0.0072(8) 0.0140(9) -0.0007(7) 0.0041(7) 0.0003(6) C69 0.0087(9) 0.0241(10) 0.0166(10) 0.0053(8) 0.0033(7) 0.0024(8) C68 0.0093(9) 0.0142(9) 0.0143(9) -0.0010(7) 0.0028(7) -0.0003(7) C4 0.0073(9) 0.0170(9) 0.0199(10) 0.0046(8) 0.0014(7) 0.0016(7) C70 0.0076(9) 0.0332(12) 0.0121(9) -0.0005(8) 0.0014(7) -0.0028(8) C1 0.0053(8) 0.0114(8) 0.0091(8) 0.0006(7) 0.0020(6) 0.0012(7) C67 0.0060(8) 0.0136(8) 0.0097(8) 0.0008(7) 0.0040(7) -0.0010(7) C66 0.0174(10) 0.0110(8) 0.0192(10) 0.0032(7) 0.0092(8) 0.0009(8) C13 0.0068(8) 0.0079(8) 0.0095(8) -0.0010(6) 0.0014(7) 0.0007(6) C18 0.0098(9) 0.0179(9) 0.0123(9) 0.0001(7) 0.0027(7) -0.0008(7) C3 0.0061(9) 0.0136(9) 0.0171(10) 0.0024(7) 0.0018(7) -0.0032(7) C71 0.0124(10) 0.0226(10) 0.0164(10) -0.0075(8) 0.0026(8) -0.0045(8) C65 0.0180(11) 0.0143(9) 0.0245(11) 0.0024(8) 0.0142(9) 0.0011(8) C17 0.0093(9) 0.0192(9) 0.0140(9) -0.0011(8) -0.0023(7) 0.0008(8) C14 0.0071(9) 0.0150(9) 0.0135(9) -0.0013(7) 0.0029(7) -0.0018(7) C2 0.0069(9) 0.0097(8) 0.0136(9) 0.0016(7) 0.0000(7) 0.0003(7) C72 0.0106(9) 0.0148(9) 0.0151(10) -0.0028(7) 0.0032(7) 0.0000(7) C61 0.0065(8) 0.0081(8) 0.0150(9) -0.0034(7) 0.0033(7) -0.0014(6) C15 0.0161(10) 0.0205(10) 0.0113(9) -0.0004(8) 0.0050(8) -0.0039(8) C16 0.0187(10) 0.0145(9) 0.0096(9) -0.0016(7) -0.0005(8) -0.0003(8) C64 0.0077(9) 0.0125(9) 0.0239(11) -0.0052(8) 0.0050(8) 0.0003(7) C62 0.0071(9) 0.0156(9) 0.0120(9) -0.0032(7) -0.0001(7) 0.0007(7) C63 0.0091(9) 0.0153(9) 0.0153(9) -0.0024(7) -0.0038(7) 0.0019(7) C33 0.0059(9) 0.0096(8) 0.0232(10) 0.0019(7) -0.0008(7) -0.0002(7) C23 0.0246(11) 0.0207(10) 0.0104(9) -0.0006(8) 0.0043(8) -0.0049(9) C52 0.0193(10) 0.0105(8) 0.0137(9) 0.0000(7) -0.0046(8) -0.0020(8) C34 0.0077(9) 0.0088(8) 0.0267(11) -0.0015(8) 0.0050(8) -0.0006(7) C24 0.0164(10) 0.0141(9) 0.0114(9) -0.0005(7) 0.0017(7) -0.0049(7) C51 0.0101(9) 0.0150(9) 0.0160(10) 0.0026(7) -0.0021(7) -0.0042(7) C53 0.0187(11) 0.0129(9) 0.0170(10) -0.0042(8) -0.0026(8) 0.0054(8) C32 0.0077(9) 0.0110(8) 0.0135(9) 0.0015(7) -0.0006(7) -0.0017(7) C35 0.0107(9) 0.0119(9) 0.0168(10) -0.0024(7) 0.0068(7) -0.0026(7) C54 0.0119(9) 0.0145(9) 0.0154(10) -0.0029(8) -0.0015(7) 0.0031(7) C22 0.0200(11) 0.0160(9) 0.0092(9) -0.0032(7) -0.0017(8) 0.0016(8) C31 0.0043(8) 0.0059(7) 0.0141(9) 0.0008(6) 0.0021(7) -0.0011(6) C50 0.0088(9) 0.0123(8) 0.0129(9) 0.0010(7) 0.0017(7) -0.0001(7) C36 0.0074(9) 0.0093(8) 0.0126(9) 0.0007(7) 0.0020(7) -0.0013(7) C49 0.0101(9) 0.0084(8) 0.0090(8) 0.0015(6) -0.0005(7) -0.0007(7) C19 0.0063(8) 0.0101(8) 0.0087(8) -0.0013(6) -0.0005(6) 0.0002(6) C42 0.0105(9) 0.0092(8) 0.0119(9) 0.0004(7) 0.0007(7) -0.0006(7) C41 0.0080(9) 0.0151(9) 0.0121(9) 0.0004(7) 0.0023(7) -0.0010(7) C21 0.0117(9) 0.0090(8) 0.0152(9) -0.0027(7) -0.0026(7) 0.0006(7) C20 0.0078(9) 0.0109(8) 0.0119(9) 0.0008(7) -0.0007(7) 0.0005(7) C37 0.0038(8) 0.0100(8) 0.0091(8) -0.0012(6) -0.0003(6) -0.0001(6) C40 0.0056(8) 0.0146(9) 0.0133(9) -0.0043(7) 0.0021(7) 0.0005(7) C25 0.0070(8) 0.0090(8) 0.0081(8) -0.0005(6) -0.0011(6) -0.0011(7) C43 0.0078(8) 0.0072(8) 0.0095(8) -0.0017(6) 0.0036(7) 0.0016(6) C38 0.0067(8) 0.0107(8) 0.0101(8) 0.0005(7) 0.0019(7) -0.0010(7) C39 0.0088(9) 0.0090(8) 0.0157(9) -0.0008(7) 0.0011(7) 0.0008(7) C30 0.0082(9) 0.0108(8) 0.0124(9) -0.0004(7) 0.0025(7) -0.0012(7) C44 0.0092(9) 0.0104(8) 0.0103(8) -0.0005(7) 0.0004(7) -0.0007(7) C26 0.0065(9) 0.0109(8) 0.0128(9) 0.0006(7) 0.0025(7) 0.0014(7) C48 0.0070(9) 0.0124(8) 0.0122(9) -0.0015(7) 0.0024(7) 0.0006(7) C45 0.0097(9) 0.0125(8) 0.0155(9) -0.0003(7) 0.0026(7) -0.0018(7) C29 0.0083(9) 0.0111(8) 0.0151(9) 0.0002(7) 0.0022(7) 0.0018(7) C27 0.0116(9) 0.0135(9) 0.0136(9) 0.0023(7) 0.0041(7) -0.0009(7) C47 0.0121(9) 0.0148(9) 0.0081(8) 0.0010(7) 0.0021(7) 0.0015(7) C46 0.0125(9) 0.0123(8) 0.0127(9) 0.0005(7) 0.0047(7) -0.0023(7) C28 0.0117(9) 0.0096(8) 0.0119(9) 0.0022(7) 0.0000(7) -0.0010(7) _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 I4 Cu1 2.6383(3) . ? I4 Cu2 2.6815(3) . ? I4 Cu4 2.6945(2) . ? I4 I1 4.23919(17) . ? I4 I2 4.4150(3) . ? I4 I3 4.4854(3) . ? I3 Cu1 2.6558(2) . ? I3 Cu3 2.6782(2) . ? I3 Cu4 2.6906(3) . ? I3 I1 4.3263(2) . ? I3 I2 4.3521(2) . ? I2 Cu3 2.6704(3) . ? I2 Cu2 2.6769(3) . ? I2 Cu1 2.6978(3) . ? I2 I1 4.5195(3) . ? I1 Cu3 2.6601(3) . ? I1 Cu2 2.6787(3) . ? I1 Cu4 2.7037(2) . ? Cu1 P1 2.2536(5) . ? Cu1 Cu2 2.7783(3) . ? Cu1 Cu4 2.7896(3) . ? Cu1 Cu3 2.7917(3) . ? Cu4 P4 2.2625(5) . ? Cu4 Cu3 2.9716(4) . ? Cu4 Cu2 3.0587(3) . ? Cu2 P2 2.2530(5) . ? Cu2 Cu3 2.7299(4) . ? Cu3 P3 2.2506(5) . ? P1 C13 1.8169(18) . ? P1 C7 1.8225(18) . ? P1 C1 1.8326(18) . ? P4 C67 1.8210(19) . ? P4 C55 1.8324(18) . ? P4 C61 1.8338(18) . ? P2 C19 1.8208(18) . ? P2 C31 1.8276(17) . ? P2 C25 1.8301(18) . ? P3 C43 1.8201(18) . ? P3 C37 1.8248(18) . ? P3 C49 1.8270(18) . ? C10 C11 1.387(3) . ? C10 C9 1.388(3) . ? C58 C59 1.385(3) . ? C58 C57 1.388(3) . ? C9 C8 1.383(2) . ? C57 C56 1.394(2) . ? C11 C12 1.393(2) . ? C59 C60 1.391(2) . ? C8 C7 1.402(2) . ? C56 C55 1.396(2) . ? C12 C7 1.394(2) . ? C5 C4 1.389(3) . ? C5 C6 1.390(3) . ? C60 C55 1.394(3) . ? C6 C1 1.389(2) . ? C69 C70 1.383(3) . ? C69 C68 1.388(3) . ? C68 C67 1.403(2) . ? C4 C3 1.382(3) . ? C70 C71 1.386(3) . ? C1 C2 1.398(2) . ? C67 C72 1.390(3) . ? C66 C65 1.391(3) . ? C66 C61 1.397(3) . ? C13 C14 1.393(2) . ? C13 C18 1.394(2) . ? C18 C17 1.384(3) . ? C3 C2 1.395(2) . ? C71 C72 1.392(3) . ? C65 C64 1.381(3) . ? C17 C16 1.388(3) . ? C14 C15 1.390(3) . ? C61 C62 1.389(3) . ? C15 C16 1.383(3) . ? C64 C63 1.380(3) . ? C62 C63 1.395(2) . ? C33 C34 1.386(3) . ? C33 C32 1.390(2) . ? C23 C22 1.381(3) . ? C23 C24 1.390(3) . ? C52 C51 1.387(3) . ? C52 C53 1.388(3) . ? C34 C35 1.386(3) . ? C24 C19 1.395(2) . ? C51 C50 1.387(3) . ? C53 C54 1.389(3) . ? C32 C31 1.394(2) . ? C35 C36 1.393(2) . ? C54 C49 1.398(2) . ? C22 C21 1.390(3) . ? C31 C36 1.401(2) . ? C50 C49 1.394(2) . ? C19 C20 1.397(2) . ? C42 C41 1.386(2) . ? C42 C37 1.397(2) . ? C41 C40 1.397(3) . ? C21 C20 1.383(3) . ? C37 C38 1.389(2) . ? C40 C39 1.382(2) . ? C25 C26 1.393(2) . ? C25 C30 1.397(2) . ? C43 C48 1.393(2) . ? C43 C44 1.394(2) . ? C38 C39 1.393(2) . ? C30 C29 1.389(2) . ? C44 C45 1.391(2) . ? C26 C27 1.393(2) . ? C48 C47 1.387(2) . ? C45 C46 1.385(3) . ? C29 C28 1.391(2) . ? C27 C28 1.385(3) . ? C47 C46 1.393(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I4 Cu2 62.962(7) . . ? Cu1 I4 Cu4 63.073(9) . . ? Cu2 I4 Cu4 69.356(8) . . ? Cu1 I4 I1 73.184(6) . . ? Cu2 I4 I1 37.711(6) . . ? Cu4 I4 I1 38.328(5) . . ? Cu1 I4 I2 34.605(6) . . ? Cu2 I4 I2 34.485(5) . . ? Cu4 I4 I2 76.767(8) . . ? I1 I4 I2 62.925(4) . . ? Cu1 I4 I3 32.204(6) . . ? Cu2 I4 I3 71.459(6) . . ? Cu4 I4 I3 33.570(5) . . ? I1 I4 I3 59.375(3) . . ? I2 I4 I3 58.540(6) . . ? Cu1 I3 Cu3 63.116(7) . . ? Cu1 I3 Cu4 62.900(9) . . ? Cu3 I3 Cu4 67.213(8) . . ? Cu1 I3 I1 71.451(6) . . ? Cu3 I3 I1 35.722(6) . . ? Cu4 I3 I1 36.780(5) . . ? Cu1 I3 I2 35.940(5) . . ? Cu3 I3 I2 35.482(5) . . ? Cu4 I3 I2 77.989(7) . . ? I1 I3 I2 62.767(4) . . ? Cu1 I3 I4 31.966(6) . . ? Cu3 I3 I4 70.261(6) . . ? Cu4 I3 I4 33.625(6) . . ? I1 I3 I4 57.478(4) . . ? I2 I3 I4 59.921(4) . . ? Cu3 I2 Cu2 61.398(9) . . ? Cu3 I2 Cu1 62.667(8) . . ? Cu2 I2 Cu1 62.250(8) . . ? Cu3 I2 I3 35.602(5) . . ? Cu2 I2 I3 73.939(8) . . ? Cu1 I2 I3 35.296(6) . . ? Cu3 I2 I4 71.593(7) . . ? Cu2 I2 I4 34.552(6) . . ? Cu1 I2 I4 33.737(6) . . ? I3 I2 I4 61.539(6) . . ? Cu3 I2 I1 31.952(6) . . ? Cu2 I2 I1 32.461(5) . . ? Cu1 I2 I1 67.724(6) . . ? I3 I2 I1 58.337(5) . . ? I4 I2 I1 56.636(4) . . ? Cu3 I1 Cu2 61.505(8) . . ? Cu3 I1 Cu4 67.279(8) . . ? Cu2 I1 Cu4 69.259(7) . . ? Cu3 I1 I4 74.916(7) . . ? Cu2 I1 I4 37.757(5) . . ? Cu4 I1 I4 38.174(5) . . ? Cu3 I1 I3 36.003(5) . . ? Cu2 I1 I3 74.402(6) . . ? Cu4 I1 I3 36.573(6) . . ? I4 I1 I3 63.147(4) . . ? Cu3 I1 I2 32.090(5) . . ? Cu2 I1 I2 32.436(6) . . ? Cu4 I1 I2 74.747(6) . . ? I4 I1 I2 60.439(4) . . ? I3 I1 I2 58.895(3) . . ? P1 Cu1 I4 105.791(15) . . ? P1 Cu1 I3 107.442(14) . . ? I4 Cu1 I3 115.830(10) . . ? P1 Cu1 I2 106.870(15) . . ? I4 Cu1 I2 111.658(9) . . ? I3 Cu1 I2 108.764(9) . . ? P1 Cu1 Cu2 143.138(15) . . ? I4 Cu1 Cu2 59.279(7) . . ? I3 Cu1 Cu2 109.344(9) . . ? I2 Cu1 Cu2 58.506(8) . . ? P1 Cu1 Cu4 138.611(15) . . ? I4 Cu1 Cu4 59.447(8) . . ? I3 Cu1 Cu4 59.160(8) . . ? I2 Cu1 Cu4 114.517(10) . . ? Cu2 Cu1 Cu4 66.644(8) . . ? P1 Cu1 Cu3 146.668(16) . . ? I4 Cu1 Cu3 107.476(9) . . ? I3 Cu1 Cu3 58.834(7) . . ? I2 Cu1 Cu3 58.186(7) . . ? Cu2 Cu1 Cu3 58.696(8) . . ? Cu4 Cu1 Cu3 64.337(8) . . ? P4 Cu4 I3 116.876(15) . . ? P4 Cu4 I4 106.465(16) . . ? I3 Cu4 I4 112.805(9) . . ? P4 Cu4 I1 109.738(14) . . ? I3 Cu4 I1 106.647(9) . . ? I4 Cu4 I1 103.498(8) . . ? P4 Cu4 Cu1 146.537(16) . . ? I3 Cu4 Cu1 57.940(7) . . ? I4 Cu4 Cu1 57.480(8) . . ? I1 Cu4 Cu1 102.902(9) . . ? P4 Cu4 Cu3 151.491(16) . . ? I3 Cu4 Cu3 56.195(8) . . ? I4 Cu4 Cu3 101.116(10) . . ? I1 Cu4 Cu3 55.661(7) . . ? Cu1 Cu4 Cu3 57.864(8) . . ? P4 Cu4 Cu2 142.389(16) . . ? I3 Cu4 Cu2 100.733(9) . . ? I4 Cu4 Cu2 55.122(6) . . ? I1 Cu4 Cu2 54.986(6) . . ? Cu1 Cu4 Cu2 56.500(8) . . ? Cu3 Cu4 Cu2 53.811(8) . . ? P2 Cu2 I2 108.030(15) . . ? P2 Cu2 I1 107.036(14) . . ? I2 Cu2 I1 115.102(10) . . ? P2 Cu2 I4 111.122(15) . . ? I2 Cu2 I4 110.963(9) . . ? I1 Cu2 I4 104.532(9) . . ? P2 Cu2 Cu3 140.698(15) . . ? I2 Cu2 Cu3 59.183(9) . . ? I1 Cu2 Cu3 58.911(7) . . ? I4 Cu2 Cu3 108.043(9) . . ? P2 Cu2 Cu1 149.022(15) . . ? I2 Cu2 Cu1 59.244(7) . . ? I1 Cu2 Cu1 103.860(9) . . ? I4 Cu2 Cu1 57.759(8) . . ? Cu3 Cu2 Cu1 60.897(8) . . ? P2 Cu2 Cu4 144.970(15) . . ? I2 Cu2 Cu4 106.988(10) . . ? I1 Cu2 Cu4 55.755(7) . . ? I4 Cu2 Cu4 55.522(7) . . ? Cu3 Cu2 Cu4 61.463(8) . . ? Cu1 Cu2 Cu4 56.856(8) . . ? P3 Cu3 I1 110.195(15) . . ? P3 Cu3 I2 107.342(15) . . ? I1 Cu3 I2 115.958(10) . . ? P3 Cu3 I3 105.670(14) . . ? I1 Cu3 I3 108.275(9) . . ? I2 Cu3 I3 108.915(8) . . ? P3 Cu3 Cu2 144.158(16) . . ? I1 Cu3 Cu2 59.584(8) . . ? I2 Cu3 Cu2 59.419(8) . . ? I3 Cu3 Cu2 110.141(9) . . ? P3 Cu3 Cu1 145.547(16) . . ? I1 Cu3 Cu1 103.991(10) . . ? I2 Cu3 Cu1 59.147(7) . . ? I3 Cu3 Cu1 58.049(7) . . ? Cu2 Cu3 Cu1 60.408(8) . . ? P3 Cu3 Cu4 142.548(15) . . ? I1 Cu3 Cu4 57.060(8) . . ? I2 Cu3 Cu4 109.682(10) . . ? I3 Cu3 Cu4 56.592(7) . . ? Cu2 Cu3 Cu4 64.726(9) . . ? Cu1 Cu3 Cu4 57.798(8) . . ? C13 P1 C7 103.26(8) . . ? C13 P1 C1 105.71(8) . . ? C7 P1 C1 105.24(8) . . ? C13 P1 Cu1 110.55(6) . . ? C7 P1 Cu1 117.07(6) . . ? C1 P1 Cu1 113.91(6) . . ? C67 P4 C55 104.17(8) . . ? C67 P4 C61 103.94(8) . . ? C55 P4 C61 101.25(8) . . ? C67 P4 Cu4 112.97(6) . . ? C55 P4 Cu4 116.48(6) . . ? C61 P4 Cu4 116.34(6) . . ? C19 P2 C31 104.23(8) . . ? C19 P2 C25 101.11(8) . . ? C31 P2 C25 105.51(8) . . ? C19 P2 Cu2 116.70(6) . . ? C31 P2 Cu2 112.79(6) . . ? C25 P2 Cu2 115.05(6) . . ? C43 P3 C37 104.75(8) . . ? C43 P3 C49 103.54(8) . . ? C37 P3 C49 103.76(8) . . ? C43 P3 Cu3 115.57(6) . . ? C37 P3 Cu3 114.42(6) . . ? C49 P3 Cu3 113.45(6) . . ? C11 C10 C9 119.89(17) . . ? C59 C58 C57 119.76(17) . . ? C8 C9 C10 120.24(17) . . ? C58 C57 C56 120.43(18) . . ? C10 C11 C12 120.08(17) . . ? C58 C59 C60 120.05(18) . . ? C9 C8 C7 120.50(17) . . ? C57 C56 C55 120.03(17) . . ? C11 C12 C7 120.41(17) . . ? C4 C5 C6 120.11(18) . . ? C12 C7 C8 118.86(16) . . ? C12 C7 P1 118.65(13) . . ? C8 C7 P1 122.47(13) . . ? C59 C60 C55 120.65(17) . . ? C1 C6 C5 120.56(17) . . ? C60 C55 C56 119.08(16) . . ? C60 C55 P4 117.16(14) . . ? C56 C55 P4 123.60(14) . . ? C70 C69 C68 120.02(19) . . ? C69 C68 C67 120.61(18) . . ? C3 C4 C5 120.05(18) . . ? C69 C70 C71 120.12(19) . . ? C6 C1 C2 118.90(16) . . ? C6 C1 P1 123.78(14) . . ? C2 C1 P1 117.31(13) . . ? C72 C67 C68 118.50(17) . . ? C72 C67 P4 121.13(14) . . ? C68 C67 P4 120.12(14) . . ? C65 C66 C61 119.72(18) . . ? C14 C13 C18 118.69(17) . . ? C14 C13 P1 122.06(14) . . ? C18 C13 P1 118.65(13) . . ? C17 C18 C13 120.84(17) . . ? C4 C3 C2 119.82(17) . . ? C70 C71 C72 119.88(19) . . ? C64 C65 C66 120.66(18) . . ? C18 C17 C16 120.18(18) . . ? C15 C14 C13 120.25(18) . . ? C3 C2 C1 120.52(17) . . ? C67 C72 C71 120.83(18) . . ? C62 C61 C66 119.26(17) . . ? C62 C61 P4 119.42(14) . . ? C66 C61 P4 121.24(14) . . ? C16 C15 C14 120.65(18) . . ? C15 C16 C17 119.37(18) . . ? C63 C64 C65 119.89(18) . . ? C61 C62 C63 120.40(18) . . ? C64 C63 C62 120.04(18) . . ? C34 C33 C32 120.55(18) . . ? C22 C23 C24 120.10(18) . . ? C51 C52 C53 119.75(18) . . ? C33 C34 C35 119.74(17) . . ? C23 C24 C19 120.27(18) . . ? C52 C51 C50 120.22(18) . . ? C52 C53 C54 120.32(18) . . ? C33 C32 C31 120.28(18) . . ? C34 C35 C36 120.08(18) . . ? C53 C54 C49 120.15(18) . . ? C23 C22 C21 120.18(18) . . ? C32 C31 C36 118.92(16) . . ? C32 C31 P2 122.10(14) . . ? C36 C31 P2 118.75(13) . . ? C51 C50 C49 120.48(18) . . ? C35 C36 C31 120.39(17) . . ? C50 C49 C54 119.07(17) . . ? C50 C49 P3 123.26(14) . . ? C54 C49 P3 117.63(14) . . ? C24 C19 C20 118.98(17) . . ? C24 C19 P2 119.67(14) . . ? C20 C19 P2 121.35(14) . . ? C41 C42 C37 120.41(17) . . ? C42 C41 C40 119.71(17) . . ? C20 C21 C22 119.87(18) . . ? C21 C20 C19 120.59(17) . . ? C38 C37 C42 119.48(16) . . ? C38 C37 P3 123.71(14) . . ? C42 C37 P3 116.80(13) . . ? C39 C40 C41 120.06(17) . . ? C26 C25 C30 118.39(16) . . ? C26 C25 P2 124.33(13) . . ? C30 C25 P2 117.28(13) . . ? C48 C43 C44 119.35(16) . . ? C48 C43 P3 122.28(14) . . ? C44 C43 P3 118.37(14) . . ? C37 C38 C39 120.09(16) . . ? C40 C39 C38 120.21(17) . . ? C29 C30 C25 120.86(17) . . ? C45 C44 C43 120.36(17) . . ? C25 C26 C27 120.86(17) . . ? C47 C48 C43 120.36(17) . . ? C46 C45 C44 119.83(18) . . ? C30 C29 C28 120.11(17) . . ? C28 C27 C26 120.15(17) . . ? C48 C47 C46 119.87(17) . . ? C45 C46 C47 120.20(17) . . ? C27 C28 C29 119.63(17) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.896 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.098 data_cuipph_mono_350k _database_code_depnum_ccdc_archive 'CCDC 777575' #TrackingRef 'mono-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method chloroform/ether _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 350(1) _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 0.0021 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 0.2614 1.2674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7268 1.8135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0905 0.0944 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 13.5817(3) _cell_length_b 27.1007(6) _cell_length_c 19.4851(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.9690(10) _cell_angle_gamma 90.00 _cell_volume 7084.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 350(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 3.057 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7252 _exptl_absorpt_correction_T_max 0.8470 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal focus sealed tube' _diffrn_source_type 'Rigaku R-AXIS' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID-F' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83348 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 30.00 _reflns_number_total 20606 _reflns_number_gt 9391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_cell_refinement 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2006), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.0414P)^2^+12.8211P] 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 20606 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1293 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.003 _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 I4 I 0.47852(3) -0.198756(15) 0.34610(2) 0.06057(11) Uani 1 1 d . . . I3 I 0.17067(3) -0.190520(16) 0.22348(3) 0.06887(13) Uani 1 1 d . . . I2 I 0.42696(3) -0.138666(15) 0.13493(2) 0.06223(12) Uani 1 1 d . . . I1 I 0.32200(3) -0.063167(14) 0.31595(2) 0.06355(12) Uani 1 1 d . . . Cu1 Cu 0.36321(6) -0.20660(3) 0.22273(5) 0.0707(2) Uani 1 1 d . . . Cu4 Cu 0.29447(6) -0.16065(3) 0.33974(5) 0.0751(2) Uani 1 1 d . . . Cu2 Cu 0.47040(6) -0.11447(3) 0.27007(5) 0.0678(2) Uani 1 1 d . . . Cu3 Cu 0.27253(6) -0.10958(3) 0.19430(5) 0.0729(2) Uani 1 1 d . . . P1 P 0.39390(11) -0.28146(6) 0.18011(9) 0.0566(4) Uani 1 1 d . . . P4 P 0.24338(13) -0.17577(6) 0.44269(10) 0.0664(4) Uani 1 1 d . . . P2 P 0.61374(11) -0.07070(6) 0.28778(9) 0.0575(4) Uani 1 1 d . . . P3 P 0.17135(12) -0.06467(6) 0.11532(9) 0.0636(4) Uani 1 1 d . . . C10 C 0.2471(7) -0.4154(4) 0.2673(6) 0.110(3) Uani 1 1 d . . . H10 H 0.2187 -0.4425 0.2861 0.132 Uiso 1 1 calc R . . C58 C 0.0770(9) -0.3227(4) 0.4585(7) 0.130(4) Uani 1 1 d . . . H58 H 0.0423 -0.3520 0.4611 0.156 Uiso 1 1 calc R . . C9 C 0.2736(7) -0.4183(3) 0.2032(6) 0.116(3) Uani 1 1 d . . . H9 H 0.2624 -0.4473 0.1777 0.140 Uiso 1 1 calc R . . C57 C 0.1171(8) -0.2999(4) 0.5163(7) 0.126(4) Uani 1 1 d . . . H57 H 0.1100 -0.3133 0.5592 0.152 Uiso 1 1 calc R . . C11 C 0.2624(8) -0.3727(4) 0.3041(6) 0.120(3) Uani 1 1 d . . . H11 H 0.2439 -0.3706 0.3480 0.144 Uiso 1 1 calc R . . C59 C 0.0861(12) -0.3036(4) 0.3955(7) 0.187(7) Uani 1 1 d . . . H59 H 0.0564 -0.3192 0.3550 0.224 Uiso 1 1 calc R . . C8 C 0.3169(6) -0.3786(3) 0.1759(4) 0.092(2) Uani 1 1 d . . . H8 H 0.3354 -0.3812 0.1320 0.110 Uiso 1 1 calc R . . C56 C 0.1704(7) -0.2556(3) 0.5131(5) 0.106(3) Uani 1 1 d . . . H56 H 0.1977 -0.2401 0.5543 0.128 Uiso 1 1 calc R . . C12 C 0.3053(6) -0.3322(3) 0.2766(4) 0.092(2) Uani 1 1 d . . . H12 H 0.3149 -0.3031 0.3020 0.110 Uiso 1 1 calc R . . C5 C 0.6646(6) -0.3507(4) 0.2329(8) 0.175(6) Uani 1 1 d . . . H5 H 0.6878 -0.3820 0.2466 0.210 Uiso 1 1 calc R . . C7 C 0.3336(4) -0.3350(2) 0.2124(4) 0.0623(15) Uani 1 1 d . . . C60 C 0.1413(9) -0.2597(4) 0.3920(5) 0.147(5) Uani 1 1 d . . . H60 H 0.1496 -0.2472 0.3488 0.176 Uiso 1 1 calc R . . C6 C 0.5627(6) -0.3417(3) 0.2184(6) 0.121(4) Uani 1 1 d . . . H6 H 0.5184 -0.3671 0.2232 0.146 Uiso 1 1 calc R . . C55 C 0.1829(5) -0.2349(2) 0.4512(4) 0.0733(18) Uani 1 1 d . . . C69 C 0.4800(9) -0.2126(6) 0.5901(8) 0.153(5) Uani 1 1 d . . . H69 H 0.5150 -0.2412 0.6048 0.184 Uiso 1 1 calc R . . C68 C 0.3985(6) -0.2157(4) 0.5376(6) 0.117(3) Uani 1 1 d . . . H68 H 0.3800 -0.2461 0.5174 0.140 Uiso 1 1 calc R . . C4 C 0.7303(6) -0.3137(4) 0.2272(6) 0.130(4) Uani 1 1 d . . . H4 H 0.7986 -0.3195 0.2369 0.156 Uiso 1 1 calc R . . C70 C 0.5092(11) -0.1699(8) 0.6197(8) 0.173(7) Uani 1 1 d . . . H70 H 0.5620 -0.1686 0.6563 0.207 Uiso 1 1 calc R . . C1 C 0.5266(4) -0.2966(2) 0.1974(3) 0.0614(15) Uani 1 1 d . . . C67 C 0.3456(5) -0.1744(3) 0.5155(4) 0.0777(19) Uani 1 1 d . . . C66 C 0.1347(8) -0.1285(3) 0.5358(6) 0.125(4) Uani 1 1 d . . . H66 H 0.1720 -0.1470 0.5708 0.150 Uiso 1 1 calc R . . C13 C 0.3557(4) -0.2854(2) 0.0873(3) 0.0626(15) Uani 1 1 d . . . C18 C 0.2572(6) -0.2808(4) 0.0611(5) 0.107(3) Uani 1 1 d . . . H18 H 0.2118 -0.2767 0.0918 0.128 Uiso 1 1 calc R . . C3 C 0.6961(5) -0.2691(3) 0.2075(5) 0.103(3) Uani 1 1 d . . . H3 H 0.7408 -0.2436 0.2038 0.123 Uiso 1 1 calc R . . C71 C 0.4608(12) -0.1284(6) 0.5959(7) 0.166(5) Uani 1 1 d . . . H71 H 0.4827 -0.0981 0.6151 0.199 Uiso 1 1 calc R . . C65 C 0.0599(10) -0.0967(4) 0.5517(8) 0.168(6) Uani 1 1 d . . . H65 H 0.0484 -0.0938 0.5973 0.202 Uiso 1 1 calc R . . C17 C 0.2224(7) -0.2818(4) -0.0080(5) 0.119(3) Uani 1 1 d . . . H17 H 0.1542 -0.2792 -0.0232 0.143 Uiso 1 1 calc R . . C14 C 0.4186(7) -0.2898(4) 0.0398(5) 0.121(3) Uani 1 1 d . . . H14 H 0.4867 -0.2929 0.0550 0.145 Uiso 1 1 calc R . . C2 C 0.5954(5) -0.2603(3) 0.1927(4) 0.083(2) Uani 1 1 d . . . H2 H 0.5734 -0.2288 0.1790 0.100 Uiso 1 1 calc R . . C72 C 0.3784(8) -0.1299(4) 0.5431(6) 0.127(3) Uani 1 1 d . . . H72 H 0.3463 -0.1009 0.5268 0.152 Uiso 1 1 calc R . . C61 C 0.1531(5) -0.1326(3) 0.4679(5) 0.078(2) Uani 1 1 d . . . C15 C 0.3836(9) -0.2896(5) -0.0304(6) 0.163(5) Uani 1 1 d . . . H15 H 0.4284 -0.2917 -0.0618 0.195 Uiso 1 1 calc R . . C16 C 0.2842(9) -0.2864(4) -0.0545(5) 0.123(3) Uani 1 1 d . . . H16 H 0.2601 -0.2875 -0.1018 0.147 Uiso 1 1 calc R . . C64 C 0.0037(8) -0.0700(4) 0.5001(9) 0.146(5) Uani 1 1 d . . . H64 H -0.0482 -0.0502 0.5102 0.175 Uiso 1 1 calc R . . C62 C 0.0990(5) -0.1036(3) 0.4191(5) 0.097(3) Uani 1 1 d . . . H62 H 0.1123 -0.1046 0.3737 0.116 Uiso 1 1 calc R . . C63 C 0.0241(7) -0.0724(4) 0.4347(7) 0.131(4) Uani 1 1 d . . . H63 H -0.0119 -0.0532 0.4000 0.158 Uiso 1 1 calc R . . C33 C 0.8760(6) -0.1458(3) 0.2851(5) 0.096(3) Uani 1 1 d . . . H33 H 0.9301 -0.1562 0.3171 0.115 Uiso 1 1 calc R . . C23 C 0.6554(11) -0.0648(6) 0.4983(5) 0.186(7) Uani 1 1 d . . . H23 H 0.6339 -0.0830 0.5336 0.224 Uiso 1 1 calc R . . C52 C -0.0105(12) -0.1646(4) -0.0480(6) 0.141(5) Uani 1 1 d . . . H52 H -0.0460 -0.1854 -0.0808 0.169 Uiso 1 1 calc R . . C34 C 0.8721(6) -0.1566(3) 0.2165(6) 0.096(3) Uani 1 1 d . . . H34 H 0.9238 -0.1741 0.2017 0.115 Uiso 1 1 calc R . . C24 C 0.6246(8) -0.0771(4) 0.4295(5) 0.133(4) Uani 1 1 d . . . H24 H 0.5806 -0.1033 0.4189 0.159 Uiso 1 1 calc R . . C51 C -0.0599(8) -0.1356(4) -0.0077(6) 0.134(4) Uani 1 1 d . . . H51 H -0.1291 -0.1367 -0.0128 0.160 Uiso 1 1 calc R . . C53 C 0.0909(11) -0.1633(4) -0.0404(6) 0.152(5) Uani 1 1 d . . . H53 H 0.1246 -0.1831 -0.0680 0.183 Uiso 1 1 calc R . . C32 C 0.8002(5) -0.1197(2) 0.3073(4) 0.0774(19) Uani 1 1 d . . . H32 H 0.8039 -0.1126 0.3543 0.093 Uiso 1 1 calc R . . C35 C 0.7925(6) -0.1417(3) 0.1694(4) 0.086(2) Uani 1 1 d . . . H35 H 0.7900 -0.1487 0.1224 0.103 Uiso 1 1 calc R . . C54 C 0.1434(8) -0.1324(4) 0.0085(5) 0.124(4) Uani 1 1 d . . . H54 H 0.2126 -0.1317 0.0136 0.148 Uiso 1 1 calc R . . C22 C 0.7182(9) -0.0253(5) 0.5137(6) 0.140(4) Uani 1 1 d . . . H22 H 0.7377 -0.0160 0.5597 0.168 Uiso 1 1 calc R . . C31 C 0.7186(4) -0.1038(2) 0.2614(4) 0.0607(15) Uani 1 1 d . . . C50 C -0.0068(6) -0.1042(3) 0.0412(5) 0.100(3) Uani 1 1 d . . . H50 H -0.0409 -0.0842 0.0683 0.119 Uiso 1 1 calc R . . C36 C 0.7152(5) -0.1161(3) 0.1922(4) 0.0745(18) Uani 1 1 d . . . H36 H 0.6600 -0.1070 0.1602 0.089 Uiso 1 1 calc R . . C49 C 0.0952(6) -0.1025(2) 0.0498(4) 0.0744(19) Uani 1 1 d . . . C19 C 0.6568(5) -0.0522(2) 0.3777(4) 0.0658(16) Uani 1 1 d . . . C42 C 0.0376(5) -0.0476(3) 0.2045(5) 0.092(2) Uani 1 1 d . . . H42 H 0.0543 -0.0796 0.2191 0.110 Uiso 1 1 calc R . . C41 C -0.0306(6) -0.0219(3) 0.2358(5) 0.106(3) Uani 1 1 d . . . H41 H -0.0606 -0.0368 0.2702 0.127 Uiso 1 1 calc R . . C21 C 0.7515(8) -0.0002(3) 0.4632(6) 0.115(3) Uani 1 1 d . . . H21 H 0.7944 0.0264 0.4739 0.137 Uiso 1 1 calc R . . C20 C 0.7220(6) -0.0137(3) 0.3952(4) 0.092(2) Uani 1 1 d . . . H20 H 0.7467 0.0035 0.3602 0.110 Uiso 1 1 calc R . . C37 C 0.0822(4) -0.0271(2) 0.1519(3) 0.0616(15) Uani 1 1 d . . . C40 C -0.0543(6) 0.0256(3) 0.2163(5) 0.092(2) Uani 1 1 d . . . H40 H -0.0990 0.0434 0.2382 0.110 Uiso 1 1 calc R . . C25 C 0.6095(4) -0.0113(2) 0.2424(3) 0.0608(15) Uani 1 1 d . . . C43 C 0.2334(5) -0.0217(2) 0.0645(4) 0.0661(16) Uani 1 1 d . . . C38 C 0.0554(5) 0.0205(2) 0.1318(4) 0.0723(18) Uani 1 1 d . . . H38 H 0.0830 0.0352 0.0961 0.087 Uiso 1 1 calc R . . C39 C -0.0119(6) 0.0467(3) 0.1641(5) 0.090(2) Uani 1 1 d . . . H39 H -0.0284 0.0789 0.1503 0.108 Uiso 1 1 calc R . . C30 C 0.5356(5) 0.0216(3) 0.2515(4) 0.083(2) Uani 1 1 d . . . H30 H 0.4880 0.0123 0.2786 0.099 Uiso 1 1 calc R . . C44 C 0.3283(5) -0.0059(3) 0.0897(4) 0.0781(19) Uani 1 1 d . . . H44 H 0.3592 -0.0170 0.1330 0.094 Uiso 1 1 calc R . . C26 C 0.6769(5) 0.0034(3) 0.2007(4) 0.082(2) Uani 1 1 d . . . H26 H 0.7277 -0.0180 0.1932 0.098 Uiso 1 1 calc R . . C48 C 0.1897(6) -0.0046(3) -0.0008(4) 0.087(2) Uani 1 1 d . . . H48 H 0.1262 -0.0154 -0.0195 0.104 Uiso 1 1 calc R . . C45 C 0.3787(7) 0.0260(3) 0.0522(5) 0.106(3) Uani 1 1 d . . . H45 H 0.4429 0.0363 0.0700 0.127 Uiso 1 1 calc R . . C29 C 0.5296(6) 0.0680(3) 0.2217(5) 0.098(3) Uani 1 1 d . . . H29 H 0.4796 0.0897 0.2297 0.117 Uiso 1 1 calc R . . C27 C 0.6704(6) 0.0495(3) 0.1697(5) 0.096(2) Uani 1 1 d . . . H27 H 0.7163 0.0585 0.1411 0.115 Uiso 1 1 calc R . . C47 C 0.2382(7) 0.0276(4) -0.0374(5) 0.104(3) Uani 1 1 d . . . H47 H 0.2070 0.0395 -0.0801 0.125 Uiso 1 1 calc R . . C46 C 0.3332(8) 0.0424(4) -0.0114(5) 0.111(3) Uani 1 1 d . . . H46 H 0.3669 0.0638 -0.0371 0.134 Uiso 1 1 calc R . . C28 C 0.5978(6) 0.0817(3) 0.1805(5) 0.092(2) Uani 1 1 d . . . H28 H 0.5944 0.1128 0.1600 0.110 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 I4 0.0564(2) 0.0630(2) 0.0588(3) 0.00496(19) -0.00184(18) 0.00228(18) I3 0.0496(2) 0.0688(3) 0.0848(3) -0.0011(2) -0.0002(2) -0.00317(18) I2 0.0619(2) 0.0656(2) 0.0585(3) -0.00028(19) 0.00716(19) 0.00738(19) I1 0.0658(2) 0.0533(2) 0.0728(3) -0.00464(19) 0.0146(2) 0.00156(18) Cu1 0.0684(5) 0.0628(5) 0.0778(6) -0.0124(4) 0.0016(4) 0.0072(4) Cu4 0.0734(5) 0.0754(5) 0.0785(6) 0.0054(4) 0.0177(4) -0.0022(4) Cu2 0.0572(4) 0.0689(5) 0.0763(6) -0.0046(4) 0.0071(4) -0.0086(4) Cu3 0.0640(5) 0.0778(5) 0.0733(6) 0.0085(4) -0.0002(4) 0.0144(4) P1 0.0521(8) 0.0525(8) 0.0638(10) -0.0034(7) 0.0050(7) 0.0006(7) P4 0.0662(10) 0.0600(9) 0.0765(12) 0.0009(8) 0.0224(9) -0.0012(8) P2 0.0527(8) 0.0600(9) 0.0587(10) 0.0005(7) 0.0051(7) -0.0077(7) P3 0.0588(9) 0.0638(9) 0.0638(11) 0.0053(8) -0.0038(8) 0.0101(8) C10 0.091(6) 0.101(7) 0.133(9) 0.028(7) 0.007(6) -0.024(5) C58 0.183(11) 0.083(6) 0.135(10) 0.009(7) 0.056(9) -0.041(7) C9 0.124(8) 0.083(6) 0.138(9) -0.003(6) 0.005(7) -0.037(5) C57 0.149(9) 0.105(7) 0.131(10) 0.025(7) 0.042(8) -0.032(7) C11 0.126(8) 0.141(9) 0.100(8) 0.033(7) 0.036(6) -0.014(7) C59 0.304(19) 0.123(9) 0.146(12) -0.036(8) 0.073(12) -0.116(11) C8 0.118(6) 0.065(4) 0.093(6) -0.007(4) 0.017(5) -0.029(4) C56 0.123(7) 0.105(6) 0.094(7) 0.008(5) 0.026(6) -0.022(6) C12 0.097(6) 0.096(6) 0.086(6) 0.008(5) 0.022(5) -0.015(5) C5 0.070(5) 0.112(7) 0.327(19) 0.107(10) -0.014(8) 0.004(5) C7 0.052(3) 0.066(4) 0.069(4) 0.001(3) 0.007(3) 0.000(3) C60 0.247(13) 0.111(7) 0.097(8) -0.025(6) 0.072(8) -0.089(8) C6 0.063(4) 0.082(5) 0.212(11) 0.059(6) -0.003(6) 0.001(4) C55 0.085(5) 0.067(4) 0.074(5) 0.006(4) 0.033(4) -0.006(4) C69 0.089(8) 0.202(14) 0.161(13) 0.038(11) -0.003(8) 0.045(8) C68 0.079(5) 0.126(8) 0.141(9) 0.017(7) 0.003(6) 0.023(5) C4 0.058(4) 0.116(7) 0.207(12) 0.061(8) -0.009(6) 0.002(5) C70 0.109(10) 0.29(2) 0.114(12) -0.023(14) -0.002(8) -0.001(13) C1 0.055(3) 0.059(3) 0.067(4) 0.009(3) 0.002(3) 0.002(3) C67 0.075(4) 0.091(5) 0.070(5) -0.003(4) 0.020(4) -0.001(4) C66 0.154(9) 0.085(6) 0.160(10) 0.033(6) 0.099(8) 0.035(6) C13 0.059(3) 0.059(3) 0.067(4) -0.001(3) 0.003(3) 0.005(3) C18 0.071(5) 0.162(9) 0.080(6) -0.026(6) -0.007(4) 0.023(5) C3 0.062(4) 0.087(5) 0.159(9) 0.031(6) 0.015(5) -0.007(4) C71 0.165(13) 0.200(15) 0.121(11) -0.049(10) -0.009(10) -0.037(11) C65 0.204(13) 0.112(8) 0.229(16) 0.031(9) 0.157(12) 0.049(9) C17 0.098(6) 0.161(9) 0.084(7) -0.021(6) -0.032(5) 0.021(6) C14 0.087(6) 0.203(11) 0.071(6) -0.012(6) 0.008(5) 0.017(6) C2 0.059(4) 0.064(4) 0.126(7) 0.015(4) 0.009(4) 0.003(3) C72 0.133(8) 0.132(9) 0.104(8) -0.022(7) -0.017(7) -0.006(7) C61 0.067(4) 0.066(4) 0.109(6) 0.006(4) 0.036(4) -0.002(3) C15 0.127(9) 0.295(18) 0.069(7) -0.029(9) 0.022(6) 0.007(10) C16 0.153(10) 0.138(8) 0.067(6) -0.009(6) -0.016(7) 0.009(7) C64 0.100(7) 0.101(8) 0.251(17) -0.013(10) 0.079(10) 0.023(6) C62 0.066(4) 0.097(6) 0.122(8) -0.022(5) -0.002(5) 0.015(4) C63 0.071(5) 0.121(8) 0.195(13) -0.027(8) -0.003(7) 0.024(5) C33 0.067(5) 0.096(6) 0.120(8) 0.004(5) -0.002(5) 0.013(4) C23 0.253(15) 0.246(15) 0.059(7) -0.017(8) 0.021(8) -0.128(13) C52 0.208(14) 0.082(6) 0.110(9) -0.019(6) -0.043(9) -0.019(8) C34 0.064(5) 0.079(5) 0.147(9) -0.013(5) 0.022(5) 0.000(4) C24 0.180(10) 0.152(9) 0.067(6) -0.012(6) 0.021(6) -0.085(8) C51 0.124(8) 0.123(8) 0.139(10) -0.004(8) -0.029(7) -0.048(7) C53 0.192(13) 0.107(8) 0.133(10) -0.043(7) -0.052(9) 0.035(8) C32 0.069(4) 0.074(4) 0.085(5) 0.007(4) -0.002(4) 0.000(4) C35 0.081(5) 0.093(5) 0.089(6) -0.012(4) 0.029(4) -0.005(4) C54 0.124(7) 0.124(8) 0.108(8) -0.030(6) -0.029(6) 0.042(6) C22 0.180(11) 0.148(10) 0.084(8) -0.044(7) -0.002(7) -0.032(9) C31 0.056(3) 0.057(3) 0.069(4) 0.004(3) 0.006(3) -0.009(3) C50 0.087(5) 0.098(6) 0.105(7) -0.008(5) -0.013(5) -0.015(5) C36 0.061(4) 0.085(5) 0.078(5) -0.001(4) 0.012(3) 0.004(3) C49 0.088(5) 0.055(4) 0.074(5) 0.001(3) -0.008(4) 0.015(3) C19 0.066(4) 0.064(4) 0.066(4) 0.002(3) 0.004(3) -0.009(3) C42 0.074(4) 0.077(5) 0.129(7) 0.014(5) 0.031(5) 0.018(4) C41 0.084(5) 0.110(7) 0.131(8) 0.025(6) 0.042(5) 0.021(5) C21 0.142(8) 0.087(6) 0.098(7) -0.026(5) -0.033(6) -0.018(6) C20 0.100(6) 0.078(5) 0.089(6) -0.003(4) -0.012(5) -0.022(4) C37 0.050(3) 0.063(4) 0.069(4) 0.008(3) 0.000(3) 0.001(3) C40 0.074(5) 0.094(6) 0.110(7) -0.014(5) 0.025(5) 0.016(4) C25 0.055(3) 0.059(3) 0.068(4) -0.001(3) 0.008(3) -0.009(3) C43 0.065(4) 0.067(4) 0.063(4) -0.006(3) 0.001(3) 0.009(3) C38 0.082(4) 0.060(4) 0.075(5) 0.007(3) 0.011(4) 0.009(3) C39 0.095(5) 0.063(4) 0.111(7) -0.006(4) 0.013(5) 0.023(4) C30 0.071(4) 0.071(4) 0.108(6) 0.011(4) 0.022(4) 0.002(4) C44 0.084(5) 0.076(4) 0.071(5) 0.001(4) 0.000(4) -0.007(4) C26 0.081(5) 0.072(4) 0.096(6) 0.010(4) 0.023(4) 0.007(4) C48 0.080(5) 0.114(6) 0.064(5) 0.012(4) 0.003(4) 0.005(4) C45 0.108(6) 0.104(6) 0.102(7) 0.007(6) 0.006(6) -0.027(5) C29 0.084(5) 0.068(5) 0.139(8) 0.007(5) 0.010(5) 0.006(4) C27 0.099(6) 0.079(5) 0.111(7) 0.026(5) 0.020(5) -0.006(5) C47 0.112(7) 0.129(7) 0.071(6) 0.028(5) 0.015(5) 0.000(6) C46 0.132(8) 0.114(7) 0.093(7) 0.018(6) 0.033(6) -0.018(6) C28 0.088(5) 0.069(5) 0.111(7) 0.019(4) -0.010(5) -0.009(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 I4 Cu1 2.6650(9) . ? I4 Cu4 2.6897(9) . ? I4 Cu2 2.7153(9) . ? I4 I1 4.2399(6) . ? I4 I2 4.3789(6) . ? I4 I3 4.4861(6) . ? I3 Cu1 2.6533(9) . ? I3 Cu3 2.7007(10) . ? I3 Cu4 2.7252(10) . ? I3 I1 4.2694(6) . ? I3 I2 4.3521(6) . ? I2 Cu3 2.6675(9) . ? I2 Cu2 2.6884(10) . ? I2 Cu1 2.7438(10) . ? I2 I1 4.4975(6) . ? I1 Cu3 2.6750(10) . ? I1 Cu2 2.7122(9) . ? I1 Cu4 2.7180(9) . ? Cu1 P1 2.2555(17) . ? Cu1 Cu4 2.8784(12) . ? Cu1 Cu3 2.9197(11) . ? Cu1 Cu2 2.9640(11) . ? Cu4 P4 2.260(2) . ? Cu4 Cu3 3.1260(13) . ? Cu4 Cu2 3.1827(11) . ? Cu2 P2 2.2599(16) . ? Cu2 Cu3 2.8604(11) . ? Cu3 P3 2.2535(18) . ? P1 C13 1.805(7) . ? P1 C7 1.825(6) . ? P1 C1 1.827(6) . ? P4 C61 1.818(7) . ? P4 C55 1.819(7) . ? P4 C67 1.824(8) . ? P2 C31 1.823(6) . ? P2 C19 1.828(7) . ? P2 C25 1.833(6) . ? P3 C37 1.810(6) . ? P3 C43 1.818(7) . ? P3 C49 1.827(7) . ? C10 C9 1.355(13) . ? C10 C11 1.361(13) . ? C58 C57 1.325(14) . ? C58 C59 1.356(15) . ? C9 C8 1.373(11) . ? C57 C56 1.408(12) . ? C11 C12 1.388(11) . ? C59 C60 1.414(12) . ? C8 C7 1.381(9) . ? C56 C55 1.366(10) . ? C12 C7 1.368(10) . ? C5 C4 1.358(12) . ? C5 C6 1.390(11) . ? C60 C55 1.379(11) . ? C6 C1 1.357(9) . ? C69 C70 1.327(18) . ? C69 C68 1.387(15) . ? C68 C67 1.364(11) . ? C4 C3 1.329(11) . ? C70 C71 1.348(19) . ? C1 C2 1.371(8) . ? C67 C72 1.367(12) . ? C66 C61 1.388(12) . ? C66 C65 1.403(12) . ? C13 C14 1.360(10) . ? C13 C18 1.362(9) . ? C18 C17 1.354(12) . ? C3 C2 1.373(9) . ? C71 C72 1.399(16) . ? C65 C64 1.371(18) . ? C17 C16 1.333(13) . ? C14 C15 1.376(13) . ? C61 C62 1.357(11) . ? C15 C16 1.361(14) . ? C64 C63 1.346(16) . ? C62 C63 1.392(12) . ? C33 C34 1.361(12) . ? C33 C32 1.373(10) . ? C23 C22 1.372(14) . ? C23 C24 1.381(13) . ? C52 C51 1.360(15) . ? C52 C53 1.362(16) . ? C34 C35 1.365(11) . ? C24 C19 1.344(10) . ? C51 C50 1.391(12) . ? C53 C54 1.380(13) . ? C32 C31 1.381(9) . ? C35 C36 1.388(9) . ? C54 C49 1.376(11) . ? C22 C21 1.332(13) . ? C31 C36 1.383(9) . ? C50 C49 1.371(10) . ? C19 C20 1.378(9) . ? C42 C41 1.375(10) . ? C42 C37 1.386(9) . ? C41 C40 1.366(11) . ? C21 C20 1.373(11) . ? C37 C38 1.382(8) . ? C40 C39 1.370(11) . ? C25 C30 1.374(9) . ? C25 C26 1.375(9) . ? C43 C44 1.375(9) . ? C43 C48 1.396(9) . ? C38 C39 1.384(9) . ? C30 C29 1.383(10) . ? C44 C45 1.381(10) . ? C26 C27 1.387(10) . ? C48 C47 1.361(11) . ? C45 C46 1.371(12) . ? C29 C28 1.369(11) . ? C27 C28 1.357(11) . ? C47 C46 1.371(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 Cu1 I4 Cu4 65.03(3) . . ? Cu1 I4 Cu2 66.85(3) . . ? Cu4 I4 Cu2 72.15(3) . . ? Cu1 I4 I1 74.499(19) . . ? Cu4 I4 I1 38.60(2) . . ? Cu2 I4 I1 38.605(18) . . ? Cu1 I4 I2 36.55(2) . . ? Cu4 I4 I2 78.61(2) . . ? Cu2 I4 I2 35.665(19) . . ? I1 I4 I2 62.885(10) . . ? Cu1 I4 I3 32.408(19) . . ? Cu4 I4 I3 34.31(2) . . ? Cu2 I4 I3 73.283(19) . . ? I1 I4 I3 58.505(9) . . ? I2 I4 I3 58.789(10) . . ? Cu1 I3 Cu3 66.09(3) . . ? Cu1 I3 Cu4 64.69(3) . . ? Cu3 I3 Cu4 70.36(3) . . ? Cu1 I3 I1 74.04(2) . . ? Cu3 I3 I1 37.21(2) . . ? Cu4 I3 I1 38.28(2) . . ? Cu1 I3 I2 36.97(2) . . ? Cu3 I3 I2 35.578(19) . . ? Cu4 I3 I2 78.80(2) . . ? I1 I3 I2 62.879(10) . . ? Cu1 I3 I4 32.57(2) . . ? Cu3 I3 I4 71.764(19) . . ? Cu4 I3 I4 33.804(19) . . ? I1 I3 I4 57.864(9) . . ? I2 I3 I4 59.376(9) . . ? Cu3 I2 Cu2 64.56(3) . . ? Cu3 I2 Cu1 65.29(3) . . ? Cu2 I2 Cu1 66.13(3) . . ? Cu3 I2 I3 36.09(2) . . ? Cu2 I2 I3 75.957(19) . . ? Cu1 I2 I3 35.559(18) . . ? Cu3 I2 I4 73.96(2) . . ? Cu2 I2 I4 36.077(19) . . ? Cu1 I2 I4 35.345(19) . . ? I3 I2 I4 61.835(10) . . ? Cu3 I2 I1 32.72(2) . . ? Cu2 I2 I1 33.784(18) . . ? Cu1 I2 I1 69.320(19) . . ? I3 I2 I1 57.662(9) . . ? I4 I2 I1 57.047(9) . . ? Cu3 I1 Cu2 64.14(3) . . ? Cu3 I1 Cu4 70.84(3) . . ? Cu2 I1 Cu4 71.76(3) . . ? Cu3 I1 I4 76.50(2) . . ? Cu2 I1 I4 38.657(19) . . ? Cu4 I1 I4 38.129(19) . . ? Cu3 I1 I3 37.63(2) . . ? Cu2 I1 I3 77.294(19) . . ? Cu4 I1 I3 38.40(2) . . ? I4 I1 I3 63.631(10) . . ? Cu3 I1 I2 32.614(19) . . ? Cu2 I1 I2 33.45(2) . . ? Cu4 I1 I2 76.14(2) . . ? I4 I1 I2 60.068(9) . . ? I3 I1 I2 59.459(10) . . ? P1 Cu1 I3 112.87(5) . . ? P1 Cu1 I4 106.71(5) . . ? I3 Cu1 I4 115.02(3) . . ? P1 Cu1 I2 106.24(5) . . ? I3 Cu1 I2 107.47(3) . . ? I4 Cu1 I2 108.10(3) . . ? P1 Cu1 Cu4 141.47(6) . . ? I3 Cu1 Cu4 58.86(3) . . ? I4 Cu1 Cu4 57.90(3) . . ? I2 Cu1 Cu4 112.11(3) . . ? P1 Cu1 Cu3 146.81(6) . . ? I3 Cu1 Cu3 57.74(2) . . ? I4 Cu1 Cu3 105.69(3) . . ? I2 Cu1 Cu3 56.09(2) . . ? Cu4 Cu1 Cu3 65.25(3) . . ? P1 Cu1 Cu2 139.67(5) . . ? I3 Cu1 Cu2 107.25(3) . . ? I4 Cu1 Cu2 57.39(2) . . ? I2 Cu1 Cu2 56.04(2) . . ? Cu4 Cu1 Cu2 66.00(3) . . ? Cu3 Cu1 Cu2 58.17(3) . . ? P4 Cu4 I4 107.53(6) . . ? P4 Cu4 I1 113.40(6) . . ? I4 Cu4 I1 103.27(3) . . ? P4 Cu4 I3 116.68(6) . . ? I4 Cu4 I3 111.88(3) . . ? I1 Cu4 I3 103.32(3) . . ? P4 Cu4 Cu1 143.80(6) . . ? I4 Cu4 Cu1 57.07(3) . . ? I1 Cu4 Cu1 102.43(3) . . ? I3 Cu4 Cu1 56.45(3) . . ? P4 Cu4 Cu3 152.37(6) . . ? I4 Cu4 Cu3 99.69(3) . . ? I1 Cu4 Cu3 53.93(2) . . ? I3 Cu4 Cu3 54.46(3) . . ? Cu1 Cu4 Cu3 58.01(3) . . ? P4 Cu4 Cu2 143.58(6) . . ? I4 Cu4 Cu2 54.30(2) . . ? I1 Cu4 Cu2 54.04(2) . . ? I3 Cu4 Cu2 99.74(3) . . ? Cu1 Cu4 Cu2 58.29(3) . . ? Cu3 Cu4 Cu2 53.92(3) . . ? P2 Cu2 I2 109.26(5) . . ? P2 Cu2 I1 110.32(5) . . ? I2 Cu2 I1 112.77(3) . . ? P2 Cu2 I4 113.42(5) . . ? I2 Cu2 I4 108.26(3) . . ? I1 Cu2 I4 102.74(3) . . ? P2 Cu2 Cu3 140.55(6) . . ? I2 Cu2 Cu3 57.36(3) . . ? I1 Cu2 Cu3 57.30(3) . . ? I4 Cu2 Cu3 106.00(3) . . ? P2 Cu2 Cu1 149.24(6) . . ? I2 Cu2 Cu1 57.83(3) . . ? I1 Cu2 Cu1 100.39(3) . . ? I4 Cu2 Cu1 55.76(2) . . ? Cu3 Cu2 Cu1 60.14(3) . . ? P2 Cu2 Cu4 145.83(6) . . ? I2 Cu2 Cu4 104.90(3) . . ? I1 Cu2 Cu4 54.20(2) . . ? I4 Cu2 Cu4 53.55(2) . . ? Cu3 Cu2 Cu4 62.03(3) . . ? Cu1 Cu2 Cu4 55.71(3) . . ? P3 Cu3 I2 107.48(6) . . ? P3 Cu3 I1 113.16(6) . . ? I2 Cu3 I1 114.67(3) . . ? P3 Cu3 I3 107.73(5) . . ? I2 Cu3 I3 108.33(3) . . ? I1 Cu3 I3 105.16(3) . . ? P3 Cu3 Cu2 143.26(6) . . ? I2 Cu3 Cu2 58.07(2) . . ? I1 Cu3 Cu2 58.56(3) . . ? I3 Cu3 Cu2 108.94(3) . . ? P3 Cu3 Cu1 144.12(6) . . ? I2 Cu3 Cu1 58.62(3) . . ? I1 Cu3 Cu1 102.42(3) . . ? I3 Cu3 Cu1 56.18(2) . . ? Cu2 Cu3 Cu1 61.69(3) . . ? P3 Cu3 Cu4 145.08(6) . . ? I2 Cu3 Cu4 106.98(3) . . ? I1 Cu3 Cu4 55.22(2) . . ? I3 Cu3 Cu4 55.19(2) . . ? Cu2 Cu3 Cu4 64.05(3) . . ? Cu1 Cu3 Cu4 56.74(3) . . ? C13 P1 C7 102.9(3) . . ? C13 P1 C1 107.0(3) . . ? C7 P1 C1 103.9(3) . . ? C13 P1 Cu1 112.4(2) . . ? C7 P1 Cu1 118.0(2) . . ? C1 P1 Cu1 111.6(2) . . ? C61 P4 C55 102.1(3) . . ? C61 P4 C67 103.9(4) . . ? C55 P4 C67 104.3(4) . . ? C61 P4 Cu4 115.9(3) . . ? C55 P4 Cu4 116.5(2) . . ? C67 P4 Cu4 112.6(2) . . ? C31 P2 C19 104.9(3) . . ? C31 P2 C25 105.2(3) . . ? C19 P2 C25 101.7(3) . . ? C31 P2 Cu2 113.03(19) . . ? C19 P2 Cu2 115.4(2) . . ? C25 P2 Cu2 115.2(2) . . ? C37 P3 C43 104.5(3) . . ? C37 P3 C49 104.5(3) . . ? C43 P3 C49 103.8(3) . . ? C37 P3 Cu3 114.1(2) . . ? C43 P3 Cu3 115.6(2) . . ? C49 P3 Cu3 113.1(2) . . ? C9 C10 C11 119.6(9) . . ? C57 C58 C59 120.6(10) . . ? C10 C9 C8 120.3(9) . . ? C58 C57 C56 120.4(10) . . ? C10 C11 C12 120.5(10) . . ? C58 C59 C60 119.2(11) . . ? C9 C8 C7 121.2(8) . . ? C55 C56 C57 121.7(9) . . ? C7 C12 C11 120.3(9) . . ? C4 C5 C6 120.0(8) . . ? C12 C7 C8 118.1(7) . . ? C12 C7 P1 118.5(6) . . ? C8 C7 P1 123.4(6) . . ? C55 C60 C59 121.5(10) . . ? C1 C6 C5 121.4(8) . . ? C56 C55 C60 116.5(7) . . ? C56 C55 P4 124.3(6) . . ? C60 C55 P4 119.0(6) . . ? C70 C69 C68 121.6(14) . . ? C67 C68 C69 120.2(11) . . ? C3 C4 C5 119.3(8) . . ? C69 C70 C71 118.8(16) . . ? C6 C1 C2 116.6(6) . . ? C6 C1 P1 123.9(5) . . ? C2 C1 P1 119.4(5) . . ? C68 C67 C72 118.5(9) . . ? C68 C67 P4 121.9(7) . . ? C72 C67 P4 119.1(7) . . ? C61 C66 C65 120.2(10) . . ? C14 C13 C18 115.9(7) . . ? C14 C13 P1 125.0(6) . . ? C18 C13 P1 118.9(6) . . ? C17 C18 C13 122.8(9) . . ? C4 C3 C2 120.8(7) . . ? C70 C71 C72 121.4(15) . . ? C64 C65 C66 120.1(12) . . ? C16 C17 C18 121.2(9) . . ? C13 C14 C15 121.3(9) . . ? C1 C2 C3 121.9(7) . . ? C67 C72 C71 119.3(11) . . ? C62 C61 C66 117.6(8) . . ? C62 C61 P4 119.9(7) . . ? C66 C61 P4 122.5(7) . . ? C16 C15 C14 120.9(10) . . ? C17 C16 C15 117.9(9) . . ? C63 C64 C65 119.7(10) . . ? C61 C62 C63 122.2(10) . . ? C64 C63 C62 120.1(12) . . ? C34 C33 C32 120.2(8) . . ? C22 C23 C24 119.0(10) . . ? C51 C52 C53 120.2(11) . . ? C33 C34 C35 120.2(8) . . ? C19 C24 C23 121.5(9) . . ? C52 C51 C50 120.0(11) . . ? C52 C53 C54 119.7(12) . . ? C33 C32 C31 121.5(8) . . ? C34 C35 C36 119.4(8) . . ? C49 C54 C53 121.3(11) . . ? C21 C22 C23 120.5(10) . . ? C32 C31 C36 117.2(6) . . ? C32 C31 P2 123.7(6) . . ? C36 C31 P2 119.0(5) . . ? C49 C50 C51 120.6(10) . . ? C31 C36 C35 121.4(7) . . ? C50 C49 C54 118.2(8) . . ? C50 C49 P3 123.7(6) . . ? C54 C49 P3 118.0(6) . . ? C24 C19 C20 117.8(7) . . ? C24 C19 P2 119.4(6) . . ? C20 C19 P2 122.8(6) . . ? C41 C42 C37 121.9(7) . . ? C40 C41 C42 120.0(8) . . ? C22 C21 C20 119.7(9) . . ? C21 C20 C19 121.3(8) . . ? C38 C37 C42 117.2(6) . . ? C38 C37 P3 125.3(5) . . ? C42 C37 P3 117.6(5) . . ? C41 C40 C39 119.5(7) . . ? C30 C25 C26 117.1(6) . . ? C30 C25 P2 118.4(5) . . ? C26 C25 P2 124.4(5) . . ? C44 C43 C48 117.7(7) . . ? C44 C43 P3 119.5(5) . . ? C48 C43 P3 122.8(5) . . ? C37 C38 C39 121.0(7) . . ? C40 C39 C38 120.4(7) . . ? C25 C30 C29 122.2(7) . . ? C43 C44 C45 121.3(8) . . ? C25 C26 C27 121.1(7) . . ? C47 C48 C43 121.3(8) . . ? C46 C45 C44 119.5(8) . . ? C28 C29 C30 119.5(8) . . ? C28 C27 C26 120.7(8) . . ? C48 C47 C46 119.9(8) . . ? C45 C46 C47 120.3(8) . . ? C27 C28 C29 119.5(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.186 _refine_diff_density_min -1.839 _refine_diff_density_rms 0.144 data_cuipph_mono_400k _database_code_depnum_ccdc_archive 'CCDC 777576' #TrackingRef 'mono-combined.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic tetrakis(triphenylphosphane-\m~3~-iodo-copper(I)) _chemical_name_common ? _chemical_formula_moiety '((C6 H5)3 P) Cu I)4' _chemical_formula_sum 'C72 H60 Cu4 I4 P4' _exptl_crystal_recrystallization_method chloroform/ether _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colorless _diffrn_ambient_temperature 400(1) _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 0.0021 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 0.2614 1.2674 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7268 1.8135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0905 0.0944 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 13.6362(8) _cell_length_b 27.2233(15) _cell_length_c 19.5261(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.9500(10) _cell_angle_gamma 90.00 _cell_volume 7160.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 400(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 3.025 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7275 _exptl_absorpt_correction_T_max 0.8485 _exptl_absorpt_process_details 'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal focus sealed tube' _diffrn_source_type 'Rigaku R-AXIS' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID-F' _diffrn_measurement_method '\w axis oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70075 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.0843 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 29.97 _reflns_number_total 20567 _reflns_number_gt 7666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_cell_refinement 'Rapid-Auto (Rigaku Co. Ltd., 2006)' _computing_data_reduction 'RAPID-AUTO (Rigaku Co. Ltd., 2006), SORTAV (Blessing, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _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^)+(0.1247P)^2^+6.2302P] 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 20567 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1996 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2796 _refine_ls_wR_factor_gt 0.1752 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.003 _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 I4 I 0.47698(5) -0.19858(2) 0.34638(4) 0.0776(2) Uani 1 1 d . . . I3 I 0.16983(5) -0.18998(3) 0.22520(4) 0.0876(2) Uani 1 1 d . . . I2 I 0.42491(5) -0.13902(2) 0.13604(4) 0.0797(2) Uani 1 1 d . . . I1 I 0.32186(5) -0.06342(2) 0.31661(4) 0.0804(2) Uani 1 1 d . . . Cu1 Cu 0.36104(10) -0.20710(5) 0.22359(8) 0.0903(4) Uani 1 1 d . . . Cu4 Cu 0.29414(11) -0.16037(5) 0.34122(8) 0.0950(4) Uani 1 1 d . . . Cu2 Cu 0.47017(9) -0.11430(5) 0.27060(8) 0.0870(4) Uani 1 1 d . . . Cu3 Cu 0.27116(10) -0.10954(5) 0.19505(8) 0.0927(4) Uani 1 1 d . . . P1 P 0.39172(18) -0.28162(9) 0.18070(14) 0.0722(6) Uani 1 1 d . . . P4 P 0.2433(2) -0.17562(11) 0.44428(17) 0.0862(8) Uani 1 1 d . . . P2 P 0.61326(19) -0.07057(10) 0.28816(15) 0.0757(7) Uani 1 1 d . . . P3 P 0.1704(2) -0.06457(10) 0.11606(15) 0.0815(7) Uani 1 1 d . . . C10 C 0.2476(12) -0.4152(7) 0.2665(11) 0.136(6) Uani 1 1 d . . . H10 H 0.2198 -0.4423 0.2852 0.163 Uiso 1 1 calc R . . C58 C 0.0770(17) -0.3217(6) 0.4577(12) 0.166(8) Uani 1 1 d . . . H58 H 0.0447 -0.3516 0.4595 0.199 Uiso 1 1 calc R . . C9 C 0.2728(13) -0.4184(6) 0.2026(10) 0.143(6) Uani 1 1 d . . . H9 H 0.2614 -0.4472 0.1769 0.171 Uiso 1 1 calc R . . C57 C 0.1118(16) -0.2982(7) 0.5142(13) 0.171(8) Uani 1 1 d . . . H57 H 0.1002 -0.3105 0.5567 0.206 Uiso 1 1 calc R . . C11 C 0.2617(14) -0.3742(9) 0.3031(9) 0.159(7) Uani 1 1 d . . . H11 H 0.2430 -0.3729 0.3468 0.191 Uiso 1 1 calc R . . C59 C 0.088(3) -0.3025(8) 0.3985(13) 0.267(17) Uani 1 1 d . . . H59 H 0.0599 -0.3183 0.3580 0.320 Uiso 1 1 calc R . . C8 C 0.3157(11) -0.3783(4) 0.1760(8) 0.117(4) Uani 1 1 d . . . H8 H 0.3335 -0.3805 0.1320 0.140 Uiso 1 1 calc R . . C56 C 0.1674(13) -0.2540(6) 0.5124(9) 0.144(6) Uani 1 1 d . . . H56 H 0.1931 -0.2386 0.5538 0.172 Uiso 1 1 calc R . . C12 C 0.3048(10) -0.3321(6) 0.2769(7) 0.116(4) Uani 1 1 d . . . H12 H 0.3136 -0.3032 0.3026 0.139 Uiso 1 1 calc R . . C5 C 0.6612(10) -0.3494(7) 0.2355(13) 0.215(12) Uani 1 1 d . . . H5 H 0.6847 -0.3801 0.2509 0.258 Uiso 1 1 calc R . . C7 C 0.3329(7) -0.3352(4) 0.2125(6) 0.083(3) Uani 1 1 d . . . C60 C 0.1412(19) -0.2587(7) 0.3927(10) 0.202(11) Uani 1 1 d . . . H60 H 0.1477 -0.2464 0.3493 0.242 Uiso 1 1 calc R . . C6 C 0.5608(10) -0.3414(5) 0.2201(10) 0.152(7) Uani 1 1 d . . . H6 H 0.5171 -0.3670 0.2247 0.183 Uiso 1 1 calc R . . C55 C 0.1834(9) -0.2341(4) 0.4520(6) 0.092(3) Uani 1 1 d . . . C69 C 0.4770(17) -0.2138(11) 0.5928(16) 0.202(11) Uani 1 1 d . . . H69 H 0.5092 -0.2424 0.6101 0.243 Uiso 1 1 calc R . . C68 C 0.3950(11) -0.2168(7) 0.5383(10) 0.156(7) Uani 1 1 d . . . H68 H 0.3753 -0.2469 0.5183 0.187 Uiso 1 1 calc R . . C4 C 0.7275(10) -0.3123(6) 0.2286(10) 0.148(7) Uani 1 1 d . . . H4 H 0.7956 -0.3178 0.2385 0.178 Uiso 1 1 calc R . . C70 C 0.5079(19) -0.1708(16) 0.6193(15) 0.213(16) Uani 1 1 d . . . H70 H 0.5622 -0.1693 0.6544 0.255 Uiso 1 1 calc R . . C1 C 0.5240(7) -0.2960(3) 0.1979(6) 0.077(3) Uani 1 1 d . . . C67 C 0.3452(9) -0.1745(5) 0.5156(6) 0.094(3) Uani 1 1 d . . . C66 C 0.1384(13) -0.1275(5) 0.5382(10) 0.152(7) Uani 1 1 d . . . H66 H 0.1776 -0.1451 0.5730 0.183 Uiso 1 1 calc R . . C13 C 0.3534(8) -0.2850(4) 0.0877(5) 0.078(3) Uani 1 1 d . . . C18 C 0.2560(10) -0.2777(6) 0.0617(8) 0.127(5) Uani 1 1 d . . . H18 H 0.2114 -0.2712 0.0920 0.152 Uiso 1 1 calc R . . C3 C 0.6928(9) -0.2691(5) 0.2076(9) 0.126(5) Uani 1 1 d . . . H3 H 0.7369 -0.2437 0.2029 0.152 Uiso 1 1 calc R . . C71 C 0.461(2) -0.1292(12) 0.5954(14) 0.213(12) Uani 1 1 d . . . H71 H 0.4827 -0.0991 0.6144 0.255 Uiso 1 1 calc R . . C65 C 0.0629(19) -0.0956(7) 0.5555(14) 0.217(13) Uani 1 1 d . . . H65 H 0.0514 -0.0924 0.6010 0.260 Uiso 1 1 calc R . . C17 C 0.2225(12) -0.2797(6) -0.0067(9) 0.141(6) Uani 1 1 d . . . H17 H 0.1548 -0.2758 -0.0216 0.169 Uiso 1 1 calc R . . C14 C 0.4152(11) -0.2922(7) 0.0418(7) 0.150(7) Uani 1 1 d . . . H14 H 0.4826 -0.2965 0.0576 0.180 Uiso 1 1 calc R . . C2 C 0.5917(8) -0.2605(4) 0.1923(7) 0.106(4) Uani 1 1 d . . . H2 H 0.5696 -0.2293 0.1777 0.127 Uiso 1 1 calc R . . C72 C 0.3807(15) -0.1313(7) 0.5429(9) 0.156(6) Uani 1 1 d . . . H72 H 0.3503 -0.1023 0.5259 0.187 Uiso 1 1 calc R . . C61 C 0.1538(9) -0.1327(4) 0.4702(7) 0.097(4) Uani 1 1 d . . . C15 C 0.3809(18) -0.2936(9) -0.0288(10) 0.193(10) Uani 1 1 d . . . H15 H 0.4256 -0.2989 -0.0594 0.231 Uiso 1 1 calc R . . C16 C 0.2812(17) -0.2870(7) -0.0546(9) 0.152(7) Uani 1 1 d . . . H16 H 0.2569 -0.2877 -0.1018 0.182 Uiso 1 1 calc R . . C64 C 0.0065(16) -0.0692(7) 0.5013(16) 0.180(11) Uani 1 1 d . . . H64 H -0.0447 -0.0490 0.5108 0.215 Uiso 1 1 calc R . . C62 C 0.0993(10) -0.1044(5) 0.4205(9) 0.122(5) Uani 1 1 d . . . H62 H 0.1113 -0.1063 0.3749 0.146 Uiso 1 1 calc R . . C63 C 0.0254(12) -0.0726(7) 0.4370(13) 0.164(8) Uani 1 1 d . . . H63 H -0.0109 -0.0537 0.4022 0.197 Uiso 1 1 calc R . . C33 C 0.8741(10) -0.1450(5) 0.2844(9) 0.117(4) Uani 1 1 d . . . H33 H 0.9279 -0.1556 0.3163 0.140 Uiso 1 1 calc R . . C23 C 0.6569(18) -0.0672(9) 0.4972(9) 0.210(11) Uani 1 1 d . . . H23 H 0.6386 -0.0870 0.5319 0.252 Uiso 1 1 calc R . . C52 C -0.010(2) -0.1633(6) -0.0472(11) 0.176(10) Uani 1 1 d . . . H52 H -0.0452 -0.1834 -0.0808 0.211 Uiso 1 1 calc R . . C34 C 0.8696(11) -0.1557(5) 0.2164(10) 0.125(5) Uani 1 1 d . . . H34 H 0.9216 -0.1729 0.2018 0.150 Uiso 1 1 calc R . . C24 C 0.6239(15) -0.0783(7) 0.4293(7) 0.162(8) Uani 1 1 d . . . H24 H 0.5782 -0.1036 0.4186 0.194 Uiso 1 1 calc R . . C51 C -0.0610(15) -0.1347(7) -0.0054(11) 0.166(7) Uani 1 1 d . . . H51 H -0.1299 -0.1362 -0.0098 0.199 Uiso 1 1 calc R . . C53 C 0.0902(19) -0.1622(7) -0.0393(11) 0.185(11) Uani 1 1 d . . . H53 H 0.1232 -0.1821 -0.0669 0.222 Uiso 1 1 calc R . . C32 C 0.7990(8) -0.1186(4) 0.3065(7) 0.102(4) Uani 1 1 d . . . H32 H 0.8037 -0.1107 0.3532 0.122 Uiso 1 1 calc R . . C35 C 0.7892(9) -0.1415(5) 0.1681(8) 0.105(4) Uani 1 1 d . . . H35 H 0.7863 -0.1490 0.1213 0.126 Uiso 1 1 calc R . . C54 C 0.1447(14) -0.1316(6) 0.0097(8) 0.146(6) Uani 1 1 d . . . H54 H 0.2136 -0.1313 0.0146 0.176 Uiso 1 1 calc R . . C22 C 0.7164(16) -0.0274(8) 0.5149(9) 0.164(8) Uani 1 1 d . . . H22 H 0.7333 -0.0181 0.5611 0.197 Uiso 1 1 calc R . . C31 C 0.7170(8) -0.1038(3) 0.2612(5) 0.076(2) Uani 1 1 d . . . C50 C -0.0074(11) -0.1043(5) 0.0423(8) 0.123(5) Uani 1 1 d . . . H50 H -0.0410 -0.0846 0.0700 0.148 Uiso 1 1 calc R . . C36 C 0.7135(8) -0.1160(4) 0.1917(6) 0.093(3) Uani 1 1 d . . . H36 H 0.6584 -0.1066 0.1601 0.111 Uiso 1 1 calc R . . C49 C 0.0965(9) -0.1018(4) 0.0508(6) 0.091(3) Uani 1 1 d . . . C19 C 0.6562(7) -0.0535(4) 0.3778(6) 0.084(3) Uani 1 1 d . . . C42 C 0.0379(9) -0.0476(5) 0.2050(8) 0.117(4) Uani 1 1 d . . . H42 H 0.0548 -0.0794 0.2199 0.140 Uiso 1 1 calc R . . C41 C -0.0299(11) -0.0216(6) 0.2362(9) 0.143(6) Uani 1 1 d . . . H41 H -0.0597 -0.0361 0.2708 0.172 Uiso 1 1 calc R . . C21 C 0.7497(13) -0.0022(6) 0.4652(10) 0.144(6) Uani 1 1 d . . . H21 H 0.7931 0.0239 0.4768 0.173 Uiso 1 1 calc R . . C20 C 0.7203(11) -0.0145(5) 0.3948(8) 0.122(4) Uani 1 1 d . . . H20 H 0.7437 0.0035 0.3602 0.146 Uiso 1 1 calc R . . C37 C 0.0813(7) -0.0274(4) 0.1518(6) 0.078(3) Uani 1 1 d . . . C40 C -0.0532(10) 0.0257(5) 0.2159(8) 0.118(4) Uani 1 1 d . . . H40 H -0.0976 0.0436 0.2375 0.142 Uiso 1 1 calc R . . C25 C 0.6096(7) -0.0121(4) 0.2432(6) 0.078(3) Uani 1 1 d . . . C43 C 0.2333(8) -0.0220(4) 0.0655(6) 0.084(3) Uani 1 1 d . . . C38 C 0.0546(9) 0.0194(4) 0.1322(6) 0.092(3) Uani 1 1 d . . . H38 H 0.0816 0.0337 0.0961 0.111 Uiso 1 1 calc R . . C39 C -0.0111(10) 0.0463(5) 0.1642(8) 0.112(4) Uani 1 1 d . . . H39 H -0.0266 0.0784 0.1503 0.135 Uiso 1 1 calc R . . C30 C 0.5360(9) 0.0212(4) 0.2519(7) 0.108(4) Uani 1 1 d . . . H30 H 0.4886 0.0120 0.2789 0.130 Uiso 1 1 calc R . . C44 C 0.3259(9) -0.0072(4) 0.0905(7) 0.099(3) Uani 1 1 d . . . H44 H 0.3569 -0.0191 0.1330 0.119 Uiso 1 1 calc R . . C26 C 0.6753(9) 0.0032(5) 0.2015(7) 0.108(4) Uani 1 1 d . . . H26 H 0.7251 -0.0182 0.1931 0.130 Uiso 1 1 calc R . . C48 C 0.1897(10) -0.0048(5) 0.0000(6) 0.109(4) Uani 1 1 d . . . H48 H 0.1267 -0.0157 -0.0192 0.131 Uiso 1 1 calc R . . C45 C 0.3779(12) 0.0266(6) 0.0531(8) 0.131(5) Uani 1 1 d . . . H45 H 0.4410 0.0374 0.0719 0.157 Uiso 1 1 calc R . . C29 C 0.5290(11) 0.0684(5) 0.2218(9) 0.123(5) Uani 1 1 d . . . H29 H 0.4787 0.0900 0.2289 0.148 Uiso 1 1 calc R . . C27 C 0.6707(12) 0.0498(5) 0.1710(8) 0.125(5) Uani 1 1 d . . . H27 H 0.7173 0.0588 0.1433 0.150 Uiso 1 1 calc R . . C47 C 0.2389(13) 0.0277(6) -0.0361(7) 0.129(5) Uani 1 1 d . . . H47 H 0.2079 0.0399 -0.0785 0.155 Uiso 1 1 calc R . . C46 C 0.3343(14) 0.0425(6) -0.0098(8) 0.132(5) Uani 1 1 d . . . H46 H 0.3685 0.0635 -0.0354 0.158 Uiso 1 1 calc R . . C28 C 0.5994(11) 0.0814(5) 0.1817(8) 0.115(4) Uani 1 1 d . . . H28 H 0.5975 0.1125 0.1617 0.137 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 I4 0.0748(4) 0.0767(4) 0.0782(4) 0.0055(3) 0.0026(3) 0.0034(3) I3 0.0666(4) 0.0832(4) 0.1097(6) -0.0036(4) 0.0037(4) -0.0038(3) I2 0.0816(4) 0.0813(4) 0.0761(4) -0.0009(3) 0.0120(3) 0.0089(3) I1 0.0856(4) 0.0667(4) 0.0907(5) -0.0052(3) 0.0193(4) 0.0017(3) Cu1 0.0884(9) 0.0790(8) 0.1012(10) -0.0141(7) 0.0073(7) 0.0093(6) Cu4 0.0962(9) 0.0940(9) 0.0982(10) 0.0073(8) 0.0264(8) -0.0005(7) Cu2 0.0754(8) 0.0885(8) 0.0962(9) -0.0062(7) 0.0110(7) -0.0125(6) Cu3 0.0859(9) 0.0962(9) 0.0931(10) 0.0106(7) 0.0052(7) 0.0201(7) P1 0.0692(14) 0.0657(13) 0.0800(17) -0.0044(12) 0.0064(12) 0.0020(11) P4 0.0874(18) 0.0778(16) 0.099(2) 0.0030(15) 0.0324(16) -0.0004(14) P2 0.0702(14) 0.0756(15) 0.0807(17) 0.0025(13) 0.0101(13) -0.0072(12) P3 0.0788(16) 0.0790(16) 0.0825(18) 0.0035(13) -0.0010(13) 0.0144(13) C10 0.133(13) 0.123(12) 0.144(16) 0.023(11) 0.001(12) -0.037(10) C58 0.23(2) 0.101(11) 0.18(2) 0.021(12) 0.070(18) -0.043(13) C9 0.165(15) 0.108(11) 0.145(15) -0.003(10) -0.006(12) -0.041(10) C57 0.20(2) 0.145(16) 0.18(2) 0.009(14) 0.073(17) -0.069(14) C11 0.161(16) 0.23(2) 0.093(11) 0.038(13) 0.030(11) -0.023(15) C59 0.49(5) 0.145(16) 0.18(2) -0.062(15) 0.12(3) -0.18(2) C8 0.153(12) 0.077(7) 0.120(10) -0.014(7) 0.021(9) -0.040(8) C56 0.176(15) 0.126(12) 0.131(13) 0.004(10) 0.031(12) -0.035(11) C12 0.129(10) 0.121(10) 0.098(10) 0.001(8) 0.022(8) -0.031(9) C5 0.068(9) 0.178(16) 0.38(3) 0.16(2) -0.016(13) 0.003(9) C7 0.073(6) 0.093(7) 0.080(7) 0.000(6) 0.004(5) 0.000(5) C60 0.35(3) 0.152(15) 0.130(15) -0.035(12) 0.111(18) -0.119(18) C6 0.093(9) 0.098(9) 0.26(2) 0.065(11) -0.007(11) 0.003(7) C55 0.114(8) 0.082(7) 0.091(8) 0.011(6) 0.046(7) -0.002(6) C69 0.117(17) 0.24(3) 0.24(3) 0.05(2) -0.013(17) 0.043(17) C68 0.098(10) 0.161(15) 0.197(19) 0.040(14) -0.010(11) 0.027(10) C4 0.068(8) 0.152(13) 0.214(19) 0.066(13) -0.014(9) 0.008(8) C70 0.115(17) 0.36(5) 0.15(2) -0.01(3) -0.008(14) -0.01(2) C1 0.076(6) 0.062(5) 0.091(7) 0.001(5) 0.000(5) 0.002(5) C67 0.096(8) 0.114(9) 0.078(7) -0.007(7) 0.026(6) -0.003(7) C66 0.187(16) 0.107(10) 0.191(17) 0.040(10) 0.117(15) 0.045(10) C13 0.080(6) 0.073(6) 0.082(7) -0.009(5) 0.014(5) 0.006(5) C18 0.084(8) 0.184(15) 0.104(10) -0.024(10) -0.011(7) 0.030(9) C3 0.078(8) 0.113(10) 0.189(16) 0.026(10) 0.024(9) 0.008(7) C71 0.19(3) 0.26(3) 0.16(2) -0.06(2) -0.033(18) -0.03(2) C65 0.29(3) 0.113(13) 0.30(3) 0.028(16) 0.21(3) 0.041(16) C17 0.108(10) 0.177(15) 0.120(13) -0.027(11) -0.038(9) 0.037(10) C14 0.101(10) 0.27(2) 0.078(9) -0.017(11) 0.005(7) 0.027(11) C2 0.081(7) 0.073(6) 0.163(12) 0.017(7) 0.019(8) 0.013(6) C72 0.172(17) 0.156(15) 0.124(14) -0.020(12) -0.027(12) -0.011(12) C61 0.096(8) 0.079(7) 0.125(10) -0.004(7) 0.048(8) -0.001(6) C15 0.19(2) 0.31(3) 0.092(13) -0.030(15) 0.039(13) 0.038(19) C16 0.195(19) 0.164(15) 0.088(11) 0.002(10) -0.009(12) 0.052(14) C64 0.161(17) 0.094(11) 0.31(3) -0.016(16) 0.12(2) 0.008(10) C62 0.095(9) 0.122(10) 0.144(13) -0.008(10) 0.008(9) 0.020(8) C63 0.099(11) 0.149(15) 0.24(2) -0.033(16) 0.007(13) 0.033(10) C33 0.081(8) 0.119(10) 0.143(13) 0.011(10) -0.005(8) 0.007(7) C23 0.28(3) 0.28(3) 0.075(11) -0.027(13) 0.019(13) -0.13(2) C52 0.27(3) 0.093(11) 0.135(16) -0.023(10) -0.051(18) -0.014(15) C34 0.090(9) 0.108(10) 0.182(17) -0.013(11) 0.035(11) -0.002(7) C24 0.24(2) 0.171(15) 0.084(10) -0.020(10) 0.054(11) -0.104(14) C51 0.145(15) 0.162(16) 0.169(18) -0.023(14) -0.042(13) -0.046(13) C53 0.23(2) 0.141(15) 0.150(17) -0.060(13) -0.071(17) 0.062(16) C32 0.072(7) 0.103(8) 0.127(10) 0.013(7) 0.004(7) 0.018(6) C35 0.089(8) 0.110(9) 0.122(11) -0.019(8) 0.032(8) -0.010(7) C54 0.155(14) 0.150(13) 0.119(12) -0.035(11) -0.025(10) 0.052(11) C22 0.21(2) 0.182(18) 0.094(12) -0.059(12) 0.015(12) -0.060(16) C31 0.084(6) 0.069(5) 0.076(7) 0.005(5) 0.014(5) -0.004(5) C50 0.116(10) 0.104(9) 0.142(13) -0.022(9) -0.007(9) -0.014(8) C36 0.076(6) 0.103(8) 0.100(9) 0.005(7) 0.017(6) 0.008(6) C49 0.101(8) 0.070(6) 0.092(8) 0.001(5) -0.019(6) 0.011(6) C19 0.071(6) 0.082(6) 0.096(8) -0.010(6) 0.002(5) -0.014(5) C42 0.095(8) 0.111(9) 0.150(13) 0.029(9) 0.037(9) 0.026(7) C41 0.125(11) 0.144(13) 0.177(16) 0.049(12) 0.077(11) 0.033(10) C21 0.155(14) 0.113(11) 0.147(15) -0.040(11) -0.032(12) -0.012(10) C20 0.153(12) 0.090(8) 0.112(11) -0.005(7) -0.010(9) -0.022(8) C37 0.069(6) 0.073(6) 0.086(7) 0.004(5) -0.004(5) 0.010(5) C40 0.112(10) 0.114(10) 0.133(12) -0.015(9) 0.031(9) 0.021(8) C25 0.070(6) 0.076(6) 0.089(7) -0.002(5) 0.009(5) -0.009(5) C43 0.082(7) 0.081(6) 0.087(7) -0.004(5) 0.010(6) 0.008(5) C38 0.108(8) 0.074(6) 0.098(8) 0.002(6) 0.022(7) 0.016(6) C39 0.119(10) 0.089(8) 0.128(11) -0.004(8) 0.015(9) 0.017(7) C30 0.093(8) 0.096(8) 0.135(11) 0.008(8) 0.018(8) 0.005(7) C44 0.105(9) 0.094(8) 0.094(8) 0.003(6) 0.004(7) 0.000(7) C26 0.109(9) 0.097(8) 0.122(10) 0.019(7) 0.030(8) 0.007(7) C48 0.114(9) 0.131(10) 0.079(8) 0.007(7) 0.005(7) -0.006(8) C45 0.149(13) 0.127(11) 0.111(12) -0.010(9) 0.004(10) -0.031(10) C29 0.115(10) 0.088(8) 0.162(14) 0.015(9) 0.008(10) 0.015(7) C27 0.133(12) 0.105(10) 0.137(13) 0.044(9) 0.026(10) -0.010(9) C47 0.139(12) 0.166(14) 0.084(9) 0.029(9) 0.018(9) 0.018(11) C46 0.167(15) 0.125(11) 0.106(12) 0.024(9) 0.032(11) -0.024(11) C28 0.107(9) 0.094(8) 0.135(12) 0.028(8) -0.005(9) -0.009(8) _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 I4 Cu1 2.6688(16) . ? I4 Cu4 2.6890(15) . ? I4 Cu2 2.7239(15) . ? I4 I1 4.2389(9) . ? I4 I2 4.3697(10) . ? I4 I3 4.4847(10) . ? I3 Cu1 2.6538(15) . ? I3 Cu3 2.7025(16) . ? I3 Cu4 2.7315(18) . ? I3 I1 4.2665(10) . ? I3 I2 4.3518(10) . ? I2 Cu3 2.6681(15) . ? I2 Cu2 2.6893(16) . ? I2 Cu1 2.7529(16) . ? I2 I1 4.4926(10) . ? I1 Cu3 2.6791(17) . ? I1 Cu2 2.7169(15) . ? I1 Cu4 2.7195(16) . ? Cu1 P1 2.259(3) . ? Cu1 Cu4 2.895(2) . ? Cu1 Cu3 2.9416(19) . ? Cu1 Cu2 3.0024(19) . ? Cu4 P4 2.266(3) . ? Cu4 Cu3 3.143(2) . ? Cu4 Cu2 3.2042(18) . ? Cu2 P2 2.266(3) . ? Cu2 Cu3 2.8830(19) . ? Cu3 P3 2.260(3) . ? P1 C13 1.812(11) . ? P1 C7 1.819(11) . ? P1 C1 1.825(10) . ? P4 C55 1.806(11) . ? P4 C67 1.807(13) . ? P4 C61 1.819(11) . ? P2 C25 1.814(11) . ? P2 C19 1.817(12) . ? P2 C31 1.824(10) . ? P3 C37 1.803(10) . ? P3 C49 1.808(11) . ? P3 C43 1.822(11) . ? C10 C11 1.32(2) . ? C10 C9 1.35(2) . ? C58 C57 1.30(3) . ? C58 C59 1.30(3) . ? C9 C8 1.377(19) . ? C57 C56 1.43(2) . ? C11 C12 1.42(2) . ? C59 C60 1.41(2) . ? C8 C7 1.375(15) . ? C56 C55 1.348(18) . ? C12 C7 1.373(16) . ? C5 C6 1.372(17) . ? C5 C4 1.38(2) . ? C60 C55 1.38(2) . ? C6 C1 1.380(15) . ? C69 C70 1.32(4) . ? C69 C68 1.42(3) . ? C68 C67 1.375(19) . ? C4 C3 1.310(18) . ? C70 C71 1.35(4) . ? C1 C2 1.353(14) . ? C67 C72 1.35(2) . ? C66 C61 1.38(2) . ? C66 C65 1.43(2) . ? C13 C14 1.337(16) . ? C13 C18 1.360(15) . ? C18 C17 1.343(19) . ? C3 C2 1.385(15) . ? C71 C72 1.38(3) . ? C65 C64 1.40(3) . ? C17 C16 1.34(2) . ? C14 C15 1.39(2) . ? C61 C62 1.363(18) . ? C15 C16 1.39(3) . ? C64 C63 1.32(3) . ? C62 C63 1.40(2) . ? C33 C34 1.35(2) . ? C33 C32 1.374(18) . ? C23 C22 1.37(2) . ? C23 C24 1.37(2) . ? C52 C53 1.35(3) . ? C52 C51 1.39(3) . ? C34 C35 1.386(19) . ? C24 C19 1.341(17) . ? C51 C50 1.37(2) . ? C53 C54 1.39(2) . ? C32 C31 1.373(15) . ? C35 C36 1.383(15) . ? C54 C49 1.379(18) . ? C22 C21 1.32(2) . ? C31 C36 1.392(15) . ? C50 C49 1.402(17) . ? C19 C20 1.384(15) . ? C42 C41 1.379(18) . ? C42 C37 1.387(16) . ? C41 C40 1.369(18) . ? C21 C20 1.41(2) . ? C37 C38 1.362(14) . ? C40 C39 1.359(18) . ? C25 C26 1.367(14) . ? C25 C30 1.382(15) . ? C43 C44 1.343(15) . ? C43 C48 1.404(16) . ? C38 C39 1.379(16) . ? C30 C29 1.411(17) . ? C44 C45 1.427(18) . ? C26 C27 1.397(17) . ? C48 C47 1.369(18) . ? C45 C46 1.351(19) . ? C29 C28 1.377(19) . ? C27 C28 1.339(19) . ? C47 C46 1.38(2) . ? 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 Cu1 I4 Cu4 65.40(5) . . ? Cu1 I4 Cu2 67.65(4) . . ? Cu4 I4 Cu2 72.59(4) . . ? Cu1 I4 I1 74.87(3) . . ? Cu4 I4 I1 38.65(3) . . ? Cu2 I4 I1 38.76(3) . . ? Cu1 I4 I2 36.96(3) . . ? Cu4 I4 I2 78.88(4) . . ? Cu2 I4 I2 35.91(3) . . ? I1 I4 I2 62.895(16) . . ? Cu1 I4 I3 32.48(3) . . ? Cu4 I4 I3 34.48(4) . . ? Cu2 I4 I3 73.70(3) . . ? I1 I4 I3 58.478(16) . . ? I2 I4 I3 58.860(16) . . ? Cu1 I3 Cu3 66.62(4) . . ? Cu1 I3 Cu4 65.01(5) . . ? Cu3 I3 Cu4 70.68(5) . . ? Cu1 I3 I1 74.48(3) . . ? Cu3 I3 I1 37.36(3) . . ? Cu4 I3 I1 38.39(3) . . ? Cu1 I3 I2 37.18(3) . . ? Cu3 I3 I2 35.61(3) . . ? Cu4 I3 I2 78.83(3) . . ? I1 I3 I2 62.828(16) . . ? Cu1 I3 I4 32.69(3) . . ? Cu3 I3 I4 71.94(3) . . ? Cu4 I3 I4 33.87(3) . . ? I1 I3 I4 57.880(15) . . ? I2 I3 I4 59.251(15) . . ? Cu3 I2 Cu2 65.11(4) . . ? Cu3 I2 Cu1 65.70(4) . . ? Cu2 I2 Cu1 66.95(4) . . ? Cu3 I2 I3 36.14(3) . . ? Cu2 I2 I3 76.42(3) . . ? Cu1 I2 I3 35.63(3) . . ? Cu3 I2 I4 74.30(3) . . ? Cu2 I2 I4 36.44(3) . . ? Cu1 I2 I4 35.65(3) . . ? I3 I2 I4 61.889(17) . . ? Cu3 I2 I1 32.92(3) . . ? Cu2 I2 I1 33.99(3) . . ? Cu1 I2 I1 69.71(3) . . ? I3 I2 I1 57.657(15) . . ? I4 I2 I1 57.130(15) . . ? Cu3 I1 Cu2 64.59(4) . . ? Cu3 I1 Cu4 71.21(5) . . ? Cu2 I1 Cu4 72.23(4) . . ? Cu3 I1 I4 76.65(3) . . ? Cu2 I1 I4 38.88(3) . . ? Cu4 I1 I4 38.14(3) . . ? Cu3 I1 I3 37.75(3) . . ? Cu2 I1 I3 77.77(3) . . ? Cu4 I1 I3 38.59(4) . . ? I4 I1 I3 63.642(17) . . ? Cu3 I1 I2 32.77(3) . . ? Cu2 I1 I2 33.60(3) . . ? Cu4 I1 I2 76.30(3) . . ? I4 I1 I2 59.976(15) . . ? I3 I1 I2 59.515(16) . . ? P1 Cu1 I3 113.65(9) . . ? P1 Cu1 I4 107.04(9) . . ? I3 Cu1 I4 114.83(6) . . ? P1 Cu1 I2 106.25(9) . . ? I3 Cu1 I2 107.19(5) . . ? I4 Cu1 I2 107.40(5) . . ? P1 Cu1 Cu4 142.03(10) . . ? I3 Cu1 Cu4 58.79(4) . . ? I4 Cu1 Cu4 57.63(4) . . ? I2 Cu1 Cu4 111.47(5) . . ? P1 Cu1 Cu3 146.77(10) . . ? I3 Cu1 Cu3 57.49(4) . . ? I4 Cu1 Cu3 105.24(5) . . ? I2 Cu1 Cu3 55.76(4) . . ? Cu4 Cu1 Cu3 65.17(5) . . ? P1 Cu1 Cu2 139.26(9) . . ? I3 Cu1 Cu2 106.84(5) . . ? I4 Cu1 Cu2 57.05(4) . . ? I2 Cu1 Cu2 55.51(4) . . ? Cu4 Cu1 Cu2 65.79(5) . . ? Cu3 Cu1 Cu2 58.02(5) . . ? P4 Cu4 I4 107.79(10) . . ? P4 Cu4 I1 113.88(9) . . ? I4 Cu4 I1 103.21(5) . . ? P4 Cu4 I3 116.52(10) . . ? I4 Cu4 I3 111.66(6) . . ? I1 Cu4 I3 103.02(5) . . ? P4 Cu4 Cu1 143.29(10) . . ? I4 Cu4 Cu1 56.96(4) . . ? I1 Cu4 Cu1 102.51(5) . . ? I3 Cu4 Cu1 56.20(4) . . ? P4 Cu4 Cu3 152.37(10) . . ? I4 Cu4 Cu3 99.51(5) . . ? I1 Cu4 Cu3 53.80(4) . . ? I3 Cu4 Cu3 54.23(4) . . ? Cu1 Cu4 Cu3 58.14(5) . . ? P4 Cu4 Cu2 143.79(11) . . ? I4 Cu4 Cu2 54.21(4) . . ? I1 Cu4 Cu2 53.85(4) . . ? I3 Cu4 Cu2 99.69(5) . . ? Cu1 Cu4 Cu2 58.72(4) . . ? Cu3 Cu4 Cu2 54.02(4) . . ? P2 Cu2 I2 109.92(9) . . ? P2 Cu2 I1 110.48(9) . . ? I2 Cu2 I1 112.41(5) . . ? P2 Cu2 I4 113.86(9) . . ? I2 Cu2 I4 107.65(5) . . ? I1 Cu2 I4 102.36(5) . . ? P2 Cu2 Cu3 140.69(9) . . ? I2 Cu2 Cu3 57.09(4) . . ? I1 Cu2 Cu3 57.07(4) . . ? I4 Cu2 Cu3 105.40(5) . . ? P2 Cu2 Cu1 149.60(9) . . ? I2 Cu2 Cu1 57.54(4) . . ? I1 Cu2 Cu1 99.85(5) . . ? I4 Cu2 Cu1 55.30(4) . . ? Cu3 Cu2 Cu1 59.94(5) . . ? P2 Cu2 Cu4 145.65(9) . . ? I2 Cu2 Cu4 104.43(5) . . ? I1 Cu2 Cu4 53.92(4) . . ? I4 Cu2 Cu4 53.20(4) . . ? Cu3 Cu2 Cu4 61.91(5) . . ? Cu1 Cu2 Cu4 55.49(4) . . ? P3 Cu3 I2 107.66(10) . . ? P3 Cu3 I1 113.36(9) . . ? I2 Cu3 I1 114.32(6) . . ? P3 Cu3 I3 108.09(10) . . ? I2 Cu3 I3 108.25(5) . . ? I1 Cu3 I3 104.89(5) . . ? P3 Cu3 Cu2 142.89(10) . . ? I2 Cu3 Cu2 57.80(4) . . ? I1 Cu3 Cu2 58.34(4) . . ? I3 Cu3 Cu2 108.94(5) . . ? P3 Cu3 Cu1 144.06(10) . . ? I2 Cu3 Cu1 58.54(4) . . ? I1 Cu3 Cu1 102.29(5) . . ? I3 Cu3 Cu1 55.90(4) . . ? Cu2 Cu3 Cu1 62.05(5) . . ? P3 Cu3 Cu4 145.33(10) . . ? I2 Cu3 Cu4 106.60(5) . . ? I1 Cu3 Cu4 54.99(4) . . ? I3 Cu3 Cu4 55.09(4) . . ? Cu2 Cu3 Cu4 64.07(5) . . ? Cu1 Cu3 Cu4 56.69(5) . . ? C13 P1 C7 103.2(5) . . ? C13 P1 C1 107.2(5) . . ? C7 P1 C1 103.9(5) . . ? C13 P1 Cu1 112.0(3) . . ? C7 P1 Cu1 118.5(4) . . ? C1 P1 Cu1 111.0(3) . . ? C55 P4 C67 104.7(6) . . ? C55 P4 C61 102.2(5) . . ? C67 P4 C61 104.1(6) . . ? C55 P4 Cu4 116.1(4) . . ? C67 P4 Cu4 112.1(4) . . ? C61 P4 Cu4 116.1(4) . . ? C25 P2 C19 102.8(5) . . ? C25 P2 C31 105.0(5) . . ? C19 P2 C31 104.8(5) . . ? C25 P2 Cu2 115.4(3) . . ? C19 P2 Cu2 114.9(3) . . ? C31 P2 Cu2 112.6(3) . . ? C37 P3 C49 104.6(5) . . ? C37 P3 C43 104.7(5) . . ? C49 P3 C43 103.5(6) . . ? C37 P3 Cu3 114.5(4) . . ? C49 P3 Cu3 112.9(3) . . ? C43 P3 Cu3 115.3(4) . . ? C11 C10 C9 121.2(17) . . ? C57 C58 C59 118.7(18) . . ? C10 C9 C8 118.9(15) . . ? C58 C57 C56 121.2(19) . . ? C10 C11 C12 121.4(16) . . ? C58 C59 C60 123(2) . . ? C7 C8 C9 121.9(14) . . ? C55 C56 C57 121.5(17) . . ? C7 C12 C11 118.0(14) . . ? C6 C5 C4 120.8(15) . . ? C12 C7 C8 118.6(12) . . ? C12 C7 P1 117.6(9) . . ? C8 C7 P1 123.8(9) . . ? C55 C60 C59 119.8(17) . . ? C5 C6 C1 120.8(13) . . ? C56 C55 C60 115.7(12) . . ? C56 C55 P4 124.4(11) . . ? C60 C55 P4 119.6(10) . . ? C70 C69 C68 121(3) . . ? C67 C68 C69 119(2) . . ? C3 C4 C5 118.5(13) . . ? C69 C70 C71 120(3) . . ? C2 C1 C6 116.5(10) . . ? C2 C1 P1 120.0(7) . . ? C6 C1 P1 123.4(9) . . ? C72 C67 C68 118.3(15) . . ? C72 C67 P4 120.3(12) . . ? C68 C67 P4 121.1(12) . . ? C61 C66 C65 120.8(18) . . ? C14 C13 C18 116.9(12) . . ? C14 C13 P1 124.4(10) . . ? C18 C13 P1 118.6(9) . . ? C17 C18 C13 121.8(14) . . ? C4 C3 C2 121.3(13) . . ? C70 C71 C72 120(3) . . ? C64 C65 C66 118(2) . . ? C16 C17 C18 123.6(15) . . ? C13 C14 C15 121.3(15) . . ? C1 C2 C3 122.0(11) . . ? C67 C72 C71 122(2) . . ? C62 C61 C66 118.6(13) . . ? C62 C61 P4 118.7(11) . . ? C66 C61 P4 122.7(12) . . ? C14 C15 C16 121.3(17) . . ? C17 C16 C15 115.1(16) . . ? C63 C64 C65 121.0(19) . . ? C61 C62 C63 121.0(17) . . ? C64 C63 C62 121(2) . . ? C34 C33 C32 119.9(14) . . ? C22 C23 C24 121.0(18) . . ? C53 C52 C51 120.6(19) . . ? C33 C34 C35 121.3(14) . . ? C19 C24 C23 121.2(15) . . ? C50 C51 C52 118.4(19) . . ? C52 C53 C54 121(2) . . ? C31 C32 C33 121.6(14) . . ? C36 C35 C34 117.8(13) . . ? C49 C54 C53 120.0(18) . . ? C21 C22 C23 118.8(16) . . ? C32 C31 C36 117.3(10) . . ? C32 C31 P2 123.4(9) . . ? C36 C31 P2 119.2(8) . . ? C51 C50 C49 122.1(16) . . ? C35 C36 C31 122.1(12) . . ? C54 C49 C50 117.9(13) . . ? C54 C49 P3 118.5(11) . . ? C50 C49 P3 123.5(10) . . ? C24 C19 C20 118.4(12) . . ? C24 C19 P2 120.0(9) . . ? C20 C19 P2 121.6(10) . . ? C41 C42 C37 121.4(12) . . ? C40 C41 C42 119.7(13) . . ? C22 C21 C20 120.9(15) . . ? C19 C20 C21 119.3(14) . . ? C38 C37 C42 117.0(10) . . ? C38 C37 P3 125.7(9) . . ? C42 C37 P3 117.3(8) . . ? C39 C40 C41 119.8(13) . . ? C26 C25 C30 115.3(11) . . ? C26 C25 P2 125.8(9) . . ? C30 C25 P2 118.8(8) . . ? C44 C43 C48 118.1(11) . . ? C44 C43 P3 119.3(9) . . ? C48 C43 P3 122.5(9) . . ? C37 C38 C39 122.3(12) . . ? C40 C39 C38 119.7(12) . . ? C25 C30 C29 123.4(12) . . ? C43 C44 C45 121.4(13) . . ? C25 C26 C27 122.8(13) . . ? C47 C48 C43 120.8(13) . . ? C46 C45 C44 119.3(14) . . ? C28 C29 C30 117.6(13) . . ? C28 C27 C26 120.2(13) . . ? C48 C47 C46 120.4(14) . . ? C45 C46 C47 119.9(14) . . ? C27 C28 C29 120.7(13) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.754 _refine_diff_density_min -1.821 _refine_diff_density_rms 0.162