# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_1 #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 4(C20H20N1P1Cu1I1) _chemical_formula_sum 'C80 H80 Cu4 I4 N4 P4' _chemical_formula_weight 1983.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.5322(5) _cell_length_b 15.6498(5) _cell_length_c 17.2181(9) _cell_angle_alpha 88.714(6) _cell_angle_beta 85.179(6) _cell_angle_gamma 81.898(5) _cell_volume 4128.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10781 _cell_measurement_theta_min 2.6246 _cell_measurement_theta_max 27.4934 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 2.632 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3528 _exptl_absorpt_correction_T_max 0.4191 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43677 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.48 _reflns_number_total 18793 _reflns_number_gt 16128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0702P)^2^+5.0559P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 18793 _refine_ls_number_parameters 873 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1256 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _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 I3 I 0.901810(18) 0.259502(18) 0.155380(15) 0.04641(8) Uani 1 1 d . . . I2 I 0.64125(2) 0.397391(19) 0.127369(16) 0.04936(8) Uani 1 1 d . . . I4 I 0.736031(19) 0.360307(17) 0.353865(14) 0.04568(8) Uani 1 1 d . . . I1 I 0.674708(18) 0.142973(17) 0.234217(16) 0.04561(8) Uani 1 1 d . . . Cu4 Cu 0.78356(4) 0.39428(4) 0.20408(3) 0.05416(14) Uani 1 1 d . . . Cu1 Cu 0.73958(4) 0.24237(4) 0.12037(3) 0.05838(15) Uani 1 1 d . . . Cu2 Cu 0.62071(4) 0.31100(4) 0.26018(3) 0.05595(14) Uani 1 1 d . . . Cu3 Cu 0.80952(4) 0.21242(4) 0.28517(3) 0.05091(13) Uani 1 1 d . . . P3 P 0.88907(7) 0.12268(7) 0.36446(6) 0.0407(2) Uani 1 1 d . . . P2 P 0.48519(7) 0.32340(7) 0.31974(6) 0.0458(2) Uani 1 1 d . . . P4 P 0.82683(8) 0.52559(7) 0.20615(7) 0.0479(2) Uani 1 1 d . . . P1 P 0.74134(8) 0.18421(8) 0.00168(7) 0.0519(3) Uani 1 1 d . . . C41 C 0.9317(3) 0.0142(3) 0.3262(2) 0.0444(9) Uani 1 1 d . . . C58 C 0.8332(3) 0.0201(3) 0.4920(2) 0.0458(9) Uani 1 1 d . . . H58 H 0.8632 -0.0277 0.4655 0.055 Uiso 1 1 calc R . . C13 C 0.6374(3) 0.1538(3) -0.0201(3) 0.0534(10) Uani 1 1 d . . . C73 C 0.9142(3) 0.5343(3) 0.2677(3) 0.0527(10) Uani 1 1 d . . . C47 C 0.9875(3) 0.1629(3) 0.3940(3) 0.0500(10) Uani 1 1 d . . . C33 C 0.4677(3) 0.2448(3) 0.3969(2) 0.0473(9) Uani 1 1 d . . . C56 C 0.7472(3) 0.0788(3) 0.6076(2) 0.0472(9) Uani 1 1 d . . . C53 C 0.8316(3) 0.1005(3) 0.4576(2) 0.0412(8) Uani 1 1 d . . . C57 C 0.7916(3) 0.0082(3) 0.5650(3) 0.0499(10) Uani 1 1 d . . . H57 H 0.7931 -0.0472 0.5860 0.060 Uiso 1 1 calc R . . C21 C 0.3980(3) 0.3109(3) 0.2581(3) 0.0550(11) Uani 1 1 d . . . C67 C 0.7373(3) 0.6085(3) 0.2428(3) 0.0599(12) Uani 1 1 d . . . C61 C 0.8608(3) 0.5696(3) 0.1103(3) 0.0565(11) Uani 1 1 d . . . C48 C 1.0045(3) 0.1702(3) 0.4705(3) 0.0605(12) Uani 1 1 d . . . H48 H 0.9660 0.1522 0.5098 0.073 Uiso 1 1 calc R . . C36 C 0.4433(3) 0.1272(3) 0.5215(3) 0.0520(10) Uani 1 1 d . . . C8 C 0.8435(3) 0.0333(3) 0.0418(3) 0.0631(13) Uani 1 1 d . . . H8 H 0.8239 0.0497 0.0925 0.076 Uiso 1 1 calc R . . C55 C 0.7452(3) 0.1602(3) 0.5724(2) 0.0518(10) Uani 1 1 d . . . H55 H 0.7161 0.2082 0.5990 0.062 Uiso 1 1 calc R . . C37 C 0.5251(3) 0.1522(3) 0.5006(3) 0.0525(10) Uani 1 1 d . . . H37 H 0.5726 0.1301 0.5280 0.063 Uiso 1 1 calc R . . C54 C 0.7853(3) 0.1709(3) 0.4989(2) 0.0485(9) Uani 1 1 d . . . H54 H 0.7815 0.2258 0.4765 0.058 Uiso 1 1 calc R . . C7 C 0.8188(3) 0.0867(3) -0.0195(3) 0.0589(12) Uani 1 1 d . . . C18 C 0.6272(4) 0.0825(3) -0.0628(3) 0.0597(12) Uani 1 1 d . . . H18 H 0.6765 0.0448 -0.0802 0.072 Uiso 1 1 calc R . . C27 C 0.4507(3) 0.4286(3) 0.3642(3) 0.0573(11) Uani 1 1 d . . . C46 C 1.0128(3) -0.0282(3) 0.3375(3) 0.0617(12) Uani 1 1 d . . . H46 H 1.0497 -0.0018 0.3660 0.074 Uiso 1 1 calc R . . C1 C 0.7689(4) 0.2580(3) -0.0780(3) 0.0611(12) Uani 1 1 d . . . C38 C 0.5359(3) 0.2100(3) 0.4391(3) 0.0507(10) Uani 1 1 d . . . H38 H 0.5910 0.2255 0.4261 0.061 Uiso 1 1 calc R . . C17 C 0.5464(4) 0.0656(3) -0.0803(3) 0.0653(14) Uani 1 1 d . . . H17 H 0.5425 0.0170 -0.1092 0.078 Uiso 1 1 calc R . . C42 C 0.8777(4) -0.0266(3) 0.2835(4) 0.0699(14) Uani 1 1 d . . . H42 H 0.8224 0.0011 0.2744 0.084 Uiso 1 1 calc R . . C35 C 0.3739(3) 0.1627(3) 0.4781(3) 0.0579(12) Uani 1 1 d . . . H35 H 0.3185 0.1476 0.4906 0.070 Uiso 1 1 calc R . . C16 C 0.4700(4) 0.1198(3) -0.0558(3) 0.0623(13) Uani 1 1 d . . . C34 C 0.3866(3) 0.2190(3) 0.4179(3) 0.0557(11) Uani 1 1 d . . . H34 H 0.3395 0.2410 0.3900 0.067 Uiso 1 1 calc R . . C78 C 0.9613(4) 0.4604(3) 0.2956(3) 0.0643(13) Uani 1 1 d . . . H78 H 0.9494 0.4071 0.2801 0.077 Uiso 1 1 calc R . . C32 C 0.4130(4) 0.4379(5) 0.4394(4) 0.0856(19) Uani 1 1 d . . . H32 H 0.4021 0.3894 0.4688 0.103 Uiso 1 1 calc R . . C74 C 0.9354(4) 0.6129(3) 0.2929(3) 0.0650(13) Uani 1 1 d . . . H74 H 0.9049 0.6644 0.2758 0.078 Uiso 1 1 calc R . . C44 C 0.9890(4) -0.1485(3) 0.2658(3) 0.0719(15) Uani 1 1 d . . . H44 H 1.0087 -0.2025 0.2445 0.086 Uiso 1 1 calc R . . C14 C 0.5614(4) 0.2053(4) 0.0074(4) 0.0771(17) Uani 1 1 d . . . H14 H 0.5657 0.2524 0.0381 0.093 Uiso 1 1 calc R . . C62 C 0.8667(5) 0.5176(4) 0.0466(3) 0.0813(18) Uani 1 1 d . . . H62 H 0.8527 0.4619 0.0531 0.098 Uiso 1 1 calc R . . C76 C 1.0467(4) 0.5410(3) 0.3715(3) 0.0639(13) Uani 1 1 d . . . C45 C 1.0413(4) -0.1097(4) 0.3074(4) 0.0737(15) Uani 1 1 d . . . H45 H 1.0966 -0.1375 0.3162 0.088 Uiso 1 1 calc R . . C9 C 0.8970(4) -0.0440(4) 0.0290(4) 0.0795(17) Uani 1 1 d . . . H9 H 0.9121 -0.0800 0.0708 0.095 Uiso 1 1 calc R . . C77 C 1.0257(4) 0.4629(3) 0.3458(4) 0.0720(16) Uani 1 1 d . . . H77 H 1.0559 0.4113 0.3629 0.086 Uiso 1 1 calc R . . C75 C 1.0000(4) 0.6159(3) 0.3423(3) 0.0696(14) Uani 1 1 d . . . H75 H 1.0130 0.6693 0.3567 0.084 Uiso 1 1 calc R . . C49 C 1.0779(4) 0.2040(4) 0.4907(4) 0.0770(17) Uani 1 1 d . . . H49 H 1.0888 0.2078 0.5427 0.092 Uiso 1 1 calc R . . C15 C 0.4797(4) 0.1895(4) -0.0090(4) 0.0838(19) Uani 1 1 d . . . H15 H 0.4305 0.2254 0.0112 0.101 Uiso 1 1 calc R . . C52 C 1.0445(3) 0.1910(4) 0.3358(4) 0.0706(15) Uani 1 1 d . . . H52 H 1.0340 0.1875 0.2837 0.085 Uiso 1 1 calc R . . C26 C 0.3233(4) 0.3687(5) 0.2537(4) 0.0843(18) Uani 1 1 d . . . H26 H 0.3163 0.4196 0.2818 0.101 Uiso 1 1 calc R . . C66 C 0.8832(5) 0.6498(4) 0.0980(4) 0.095(2) Uani 1 1 d . . . H66 H 0.8803 0.6865 0.1401 0.114 Uiso 1 1 calc R . . C43 C 0.9056(5) -0.1079(4) 0.2545(4) 0.0830(18) Uani 1 1 d . . . H43 H 0.8685 -0.1357 0.2273 0.100 Uiso 1 1 calc R . . C50 C 1.1341(4) 0.2316(4) 0.4319(6) 0.089(2) Uani 1 1 d . . . H50 H 1.1830 0.2549 0.4444 0.107 Uiso 1 1 calc R . . C22 C 0.4036(4) 0.2366(4) 0.2167(4) 0.0809(17) Uani 1 1 d . . . H22 H 0.4529 0.1956 0.2187 0.097 Uiso 1 1 calc R . . C23 C 0.3375(5) 0.2207(5) 0.1715(4) 0.095(2) Uani 1 1 d . . . H23 H 0.3432 0.1690 0.1448 0.113 Uiso 1 1 calc R . . C12 C 0.8515(4) 0.0617(4) -0.0945(3) 0.0752(16) Uani 1 1 d . . . H12 H 0.8366 0.0974 -0.1366 0.090 Uiso 1 1 calc R . . C68 C 0.6790(4) 0.6480(5) 0.1933(4) 0.0877(19) Uani 1 1 d . . . H68 H 0.6853 0.6347 0.1406 0.105 Uiso 1 1 calc R . . N3 N 0.7060(3) 0.0689(3) 0.6805(2) 0.0696(12) Uani 1 1 d . . . N2 N 0.4309(3) 0.0693(3) 0.5816(3) 0.0728(13) Uani 1 1 d . . . N1 N 0.3892(4) 0.1052(4) -0.0744(3) 0.0829(15) Uani 1 1 d . . . N4 N 1.1112(4) 0.5444(3) 0.4206(4) 0.0968(19) Uani 1 1 d . . . C40 C 0.5016(4) 0.0319(4) 0.6258(3) 0.0771(16) Uani 1 1 d . . . H40A H 0.5527 0.0158 0.5911 0.116 Uiso 1 1 calc R . . H40B H 0.4858 -0.0184 0.6533 0.116 Uiso 1 1 calc R . . H40C H 0.5134 0.0733 0.6624 0.116 Uiso 1 1 calc R . . C28 C 0.4676(4) 0.5015(4) 0.3231(4) 0.0819(18) Uani 1 1 d . . . H28 H 0.4952 0.4965 0.2730 0.098 Uiso 1 1 calc R . . C11 C 0.9054(5) -0.0149(4) -0.1073(4) 0.087(2) Uani 1 1 d . . . H11 H 0.9267 -0.0308 -0.1578 0.105 Uiso 1 1 calc R . . C59 C 0.7112(5) -0.0149(4) 0.7177(3) 0.089(2) Uani 1 1 d . . . H59A H 0.6863 -0.0535 0.6863 0.133 Uiso 1 1 calc R . . H59B H 0.6794 -0.0100 0.7681 0.133 Uiso 1 1 calc R . . H59C H 0.7711 -0.0371 0.7235 0.133 Uiso 1 1 calc R . . C10 C 0.9280(4) -0.0679(4) -0.0460(5) 0.087(2) Uani 1 1 d . . . H10 H 0.9642 -0.1199 -0.0548 0.105 Uiso 1 1 calc R . . C51 C 1.1186(4) 0.2250(4) 0.3569(5) 0.086(2) Uani 1 1 d . . . H51 H 1.1574 0.2432 0.3180 0.103 Uiso 1 1 calc R . . C64 C 0.9135(4) 0.6273(6) -0.0366(5) 0.100(3) Uani 1 1 d . . . H64 H 0.9300 0.6473 -0.0862 0.121 Uiso 1 1 calc R . . C2 C 0.8508(4) 0.2836(5) -0.0839(4) 0.0851(18) Uani 1 1 d . . . H2 H 0.8911 0.2618 -0.0489 0.102 Uiso 1 1 calc R . . C39 C 0.3432(5) 0.0529(6) 0.6073(4) 0.109(3) Uani 1 1 d . . . H39A H 0.3092 0.1054 0.6263 0.164 Uiso 1 1 calc R . . H39B H 0.3459 0.0102 0.6483 0.164 Uiso 1 1 calc R . . H39C H 0.3167 0.0323 0.5643 0.164 Uiso 1 1 calc R . . C30 C 0.4048(6) 0.5909(6) 0.4311(6) 0.115(3) Uani 1 1 d . . . H30 H 0.3883 0.6450 0.4531 0.138 Uiso 1 1 calc R . . C72 C 0.7245(5) 0.6267(4) 0.3222(4) 0.0851(18) Uani 1 1 d . . . H72 H 0.7625 0.5985 0.3565 0.102 Uiso 1 1 calc R . . C19 C 0.3814(5) 0.0364(5) -0.1271(4) 0.099(2) Uani 1 1 d . . . H19A H 0.4152 0.0443 -0.1754 0.149 Uiso 1 1 calc R . . H19B H 0.3213 0.0375 -0.1368 0.149 Uiso 1 1 calc R . . H19C H 0.4026 -0.0181 -0.1041 0.149 Uiso 1 1 calc R . . C60 C 0.6731(5) 0.1419(4) 0.7268(3) 0.089(2) Uani 1 1 d . . . H60A H 0.7189 0.1760 0.7324 0.134 Uiso 1 1 calc R . . H60B H 0.6515 0.1231 0.7773 0.134 Uiso 1 1 calc R . . H60C H 0.6265 0.1760 0.7022 0.134 Uiso 1 1 calc R . . C6 C 0.7108(6) 0.2918(5) -0.1284(4) 0.098(2) Uani 1 1 d . . . H6 H 0.6554 0.2751 -0.1252 0.117 Uiso 1 1 calc R . . C70 C 0.6005(6) 0.7298(5) 0.3000(6) 0.113(3) Uani 1 1 d . . . H70 H 0.5569 0.7734 0.3181 0.136 Uiso 1 1 calc R . . C3 C 0.8729(6) 0.3407(5) -0.1406(5) 0.107(3) Uani 1 1 d . . . H3 H 0.9284 0.3572 -0.1439 0.129 Uiso 1 1 calc R . . C24 C 0.2667(5) 0.2775(6) 0.1657(4) 0.101(2) Uani 1 1 d . . . H24 H 0.2239 0.2668 0.1339 0.121 Uiso 1 1 calc R . . C63 C 0.8928(6) 0.5456(6) -0.0269(4) 0.109(3) Uani 1 1 d . . . H63 H 0.8963 0.5093 -0.0694 0.131 Uiso 1 1 calc R . . C25 C 0.2573(5) 0.3524(6) 0.2073(5) 0.109(3) Uani 1 1 d . . . H25 H 0.2072 0.3923 0.2048 0.131 Uiso 1 1 calc R . . C65 C 0.9101(6) 0.6786(5) 0.0246(5) 0.106(3) Uani 1 1 d . . . H65 H 0.9259 0.7336 0.0180 0.127 Uiso 1 1 calc R . . C80 C 1.1494(6) 0.4680(5) 0.4583(5) 0.115(3) Uani 1 1 d . . . H80A H 1.1043 0.4405 0.4859 0.172 Uiso 1 1 calc R . . H80B H 1.1886 0.4827 0.4944 0.172 Uiso 1 1 calc R . . H80C H 1.1809 0.4293 0.4200 0.172 Uiso 1 1 calc R . . C31 C 0.3914(6) 0.5191(6) 0.4713(5) 0.113(3) Uani 1 1 d . . . H31 H 0.3668 0.5241 0.5224 0.135 Uiso 1 1 calc R . . C29 C 0.4437(6) 0.5823(5) 0.3559(6) 0.109(3) Uani 1 1 d . . . H29 H 0.4539 0.6314 0.3270 0.130 Uiso 1 1 calc R . . C79 C 1.1334(6) 0.6255(5) 0.4445(6) 0.131(4) Uani 1 1 d . . . H79A H 1.1159 0.6695 0.4070 0.197 Uiso 1 1 calc R . . H79B H 1.1952 0.6206 0.4479 0.197 Uiso 1 1 calc R . . H79C H 1.1037 0.6406 0.4945 0.197 Uiso 1 1 calc R . . C20 C 0.3091(5) 0.1581(6) -0.0454(5) 0.107(3) Uani 1 1 d . . . H20A H 0.2959 0.1445 0.0086 0.160 Uiso 1 1 calc R . . H20B H 0.2621 0.1469 -0.0748 0.160 Uiso 1 1 calc R . . H20C H 0.3162 0.2180 -0.0507 0.160 Uiso 1 1 calc R . . C71 C 0.6552(6) 0.6867(5) 0.3498(5) 0.113(3) Uani 1 1 d . . . H71 H 0.6460 0.6976 0.4029 0.135 Uiso 1 1 calc R . . C4 C 0.8159(8) 0.3735(5) -0.1920(5) 0.120(3) Uani 1 1 d . . . H4 H 0.8324 0.4107 -0.2316 0.144 Uiso 1 1 calc R . . C69 C 0.6101(5) 0.7085(6) 0.2232(6) 0.120(3) Uani 1 1 d . . . H69 H 0.5700 0.7348 0.1899 0.144 Uiso 1 1 calc R . . C5 C 0.7334(8) 0.3515(6) -0.1853(5) 0.138(4) Uani 1 1 d . . . H5 H 0.6924 0.3764 -0.2185 0.166 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 I3 0.04431(15) 0.04894(15) 0.04416(14) -0.00071(11) 0.00676(11) -0.00631(11) I2 0.05511(17) 0.04930(16) 0.04440(14) 0.00276(11) -0.00803(12) -0.00793(12) I4 0.05876(17) 0.04099(14) 0.03622(13) -0.00397(10) -0.00137(11) -0.00412(12) I1 0.04948(16) 0.03867(14) 0.04908(15) -0.00303(10) -0.00152(11) -0.00862(11) Cu4 0.0648(4) 0.0467(3) 0.0534(3) -0.0005(2) -0.0050(3) -0.0163(3) Cu1 0.0636(4) 0.0647(4) 0.0474(3) -0.0121(3) -0.0030(3) -0.0098(3) Cu2 0.0526(3) 0.0555(3) 0.0567(3) -0.0010(2) 0.0109(3) -0.0056(3) Cu3 0.0548(3) 0.0490(3) 0.0472(3) 0.0036(2) -0.0039(2) -0.0019(2) P3 0.0410(5) 0.0394(5) 0.0408(5) 0.0019(4) -0.0017(4) -0.0044(4) P2 0.0437(6) 0.0480(6) 0.0434(5) -0.0002(4) 0.0045(4) -0.0033(5) P4 0.0533(6) 0.0391(5) 0.0525(6) 0.0024(4) -0.0059(5) -0.0105(5) P1 0.0570(7) 0.0559(7) 0.0422(5) -0.0111(5) 0.0006(5) -0.0072(5) C41 0.049(2) 0.040(2) 0.042(2) 0.0012(16) 0.0022(17) -0.0037(17) C58 0.047(2) 0.041(2) 0.050(2) -0.0001(17) -0.0032(18) -0.0055(17) C13 0.062(3) 0.054(3) 0.045(2) -0.0106(19) -0.003(2) -0.009(2) C73 0.058(3) 0.041(2) 0.061(3) -0.0013(19) -0.010(2) -0.011(2) C47 0.041(2) 0.040(2) 0.068(3) 0.0048(19) -0.0023(19) -0.0049(17) C33 0.044(2) 0.055(2) 0.042(2) 0.0033(17) -0.0019(17) -0.0066(19) C56 0.044(2) 0.057(3) 0.041(2) 0.0088(18) -0.0051(17) -0.0089(19) C53 0.039(2) 0.043(2) 0.0418(19) 0.0034(16) -0.0046(15) -0.0082(16) C57 0.054(2) 0.046(2) 0.051(2) 0.0111(18) -0.0066(19) -0.0123(19) C21 0.056(3) 0.064(3) 0.043(2) 0.007(2) -0.0008(19) -0.007(2) C67 0.063(3) 0.046(2) 0.070(3) 0.000(2) -0.001(2) -0.012(2) C61 0.052(3) 0.055(3) 0.063(3) 0.011(2) -0.006(2) -0.011(2) C48 0.054(3) 0.058(3) 0.070(3) -0.014(2) -0.011(2) -0.007(2) C36 0.055(3) 0.056(3) 0.047(2) 0.0029(19) -0.0038(19) -0.015(2) C8 0.062(3) 0.059(3) 0.066(3) -0.009(2) 0.009(2) -0.009(2) C55 0.056(3) 0.051(2) 0.044(2) 0.0015(18) 0.0011(19) 0.004(2) C37 0.046(2) 0.060(3) 0.053(2) 0.005(2) -0.0115(19) -0.009(2) C54 0.052(2) 0.046(2) 0.045(2) 0.0011(17) 0.0003(18) -0.0027(19) C7 0.060(3) 0.060(3) 0.057(3) -0.012(2) 0.004(2) -0.009(2) C18 0.075(3) 0.055(3) 0.050(2) -0.013(2) 0.005(2) -0.016(2) C27 0.049(2) 0.057(3) 0.064(3) -0.008(2) 0.002(2) 0.000(2) C46 0.052(3) 0.057(3) 0.074(3) -0.007(2) -0.010(2) 0.002(2) C1 0.078(3) 0.057(3) 0.047(2) -0.006(2) 0.004(2) -0.008(2) C38 0.040(2) 0.062(3) 0.052(2) -0.002(2) -0.0007(18) -0.015(2) C17 0.090(4) 0.060(3) 0.050(3) -0.015(2) 0.001(2) -0.029(3) C42 0.066(3) 0.052(3) 0.091(4) -0.013(3) -0.021(3) 0.003(2) C35 0.043(2) 0.075(3) 0.058(3) 0.015(2) -0.004(2) -0.016(2) C16 0.073(3) 0.064(3) 0.055(3) -0.005(2) -0.010(2) -0.025(3) C34 0.037(2) 0.075(3) 0.055(3) 0.012(2) -0.0028(18) -0.010(2) C78 0.070(3) 0.040(2) 0.087(4) -0.005(2) -0.027(3) -0.010(2) C32 0.088(4) 0.087(4) 0.075(4) -0.027(3) 0.017(3) 0.003(3) C74 0.082(4) 0.042(2) 0.076(3) 0.002(2) -0.023(3) -0.016(2) C44 0.091(4) 0.047(3) 0.069(3) -0.008(2) 0.005(3) 0.013(3) C14 0.067(3) 0.072(4) 0.097(4) -0.042(3) -0.016(3) -0.013(3) C62 0.109(5) 0.072(4) 0.061(3) 0.010(3) 0.008(3) -0.018(3) C76 0.066(3) 0.058(3) 0.072(3) -0.004(2) -0.020(3) -0.015(2) C45 0.060(3) 0.067(3) 0.087(4) -0.012(3) 0.000(3) 0.012(3) C9 0.071(4) 0.066(3) 0.097(5) 0.002(3) 0.007(3) 0.000(3) C77 0.069(3) 0.045(3) 0.106(4) -0.004(3) -0.036(3) -0.006(2) C75 0.089(4) 0.048(3) 0.079(4) -0.002(2) -0.025(3) -0.023(3) C49 0.057(3) 0.064(3) 0.112(5) -0.028(3) -0.022(3) -0.003(3) C15 0.066(3) 0.075(4) 0.114(5) -0.039(4) -0.018(3) -0.009(3) C52 0.051(3) 0.067(3) 0.093(4) 0.024(3) -0.001(3) -0.011(2) C26 0.072(4) 0.083(4) 0.096(5) -0.001(3) -0.025(3) 0.004(3) C66 0.126(6) 0.078(4) 0.092(5) 0.028(4) -0.020(4) -0.048(4) C43 0.100(5) 0.052(3) 0.099(5) -0.020(3) -0.030(4) -0.004(3) C50 0.050(3) 0.052(3) 0.169(8) -0.001(4) -0.027(4) -0.010(2) C22 0.083(4) 0.088(4) 0.072(4) -0.011(3) -0.021(3) -0.003(3) C23 0.109(6) 0.102(5) 0.080(4) -0.008(4) -0.028(4) -0.026(5) C12 0.086(4) 0.077(4) 0.057(3) -0.014(3) 0.013(3) 0.000(3) C68 0.076(4) 0.096(5) 0.084(4) -0.006(4) -0.010(3) 0.016(4) N3 0.082(3) 0.074(3) 0.048(2) 0.010(2) 0.010(2) -0.007(2) N2 0.067(3) 0.087(3) 0.070(3) 0.032(2) -0.018(2) -0.029(2) N1 0.090(4) 0.083(3) 0.087(3) -0.015(3) -0.025(3) -0.041(3) N4 0.111(4) 0.066(3) 0.126(5) -0.005(3) -0.070(4) -0.018(3) C40 0.096(4) 0.070(4) 0.069(3) 0.015(3) -0.026(3) -0.016(3) C28 0.086(4) 0.056(3) 0.097(4) -0.003(3) 0.019(3) 0.000(3) C11 0.095(5) 0.080(4) 0.078(4) -0.030(3) 0.031(3) 0.000(4) C59 0.111(5) 0.091(4) 0.059(3) 0.024(3) 0.014(3) -0.011(4) C10 0.074(4) 0.059(3) 0.120(6) -0.019(4) 0.024(4) 0.002(3) C51 0.051(3) 0.068(4) 0.137(6) 0.032(4) 0.000(4) -0.013(3) C64 0.072(4) 0.143(7) 0.089(5) 0.054(5) -0.007(4) -0.031(4) C2 0.079(4) 0.094(5) 0.078(4) 0.008(3) 0.018(3) -0.018(3) C39 0.086(5) 0.154(7) 0.098(5) 0.063(5) -0.013(4) -0.061(5) C30 0.103(6) 0.080(5) 0.157(8) -0.056(6) -0.023(6) 0.019(4) C72 0.094(5) 0.084(4) 0.072(4) -0.011(3) 0.008(3) -0.004(4) C19 0.119(6) 0.107(5) 0.089(5) -0.023(4) -0.025(4) -0.059(5) C60 0.113(5) 0.090(5) 0.058(3) 0.000(3) 0.020(3) -0.005(4) C6 0.111(6) 0.090(5) 0.100(5) 0.024(4) -0.024(4) -0.032(4) C70 0.106(6) 0.077(5) 0.140(8) -0.012(5) 0.026(5) 0.023(4) C3 0.106(6) 0.097(6) 0.112(6) 0.004(5) 0.037(5) -0.020(5) C24 0.093(5) 0.131(7) 0.086(5) 0.007(5) -0.042(4) -0.023(5) C63 0.138(7) 0.115(6) 0.073(4) 0.018(4) 0.015(4) -0.025(5) C25 0.086(5) 0.130(7) 0.111(6) 0.026(5) -0.038(4) 0.002(5) C65 0.130(7) 0.096(5) 0.104(6) 0.042(5) -0.028(5) -0.060(5) C80 0.114(6) 0.093(5) 0.149(7) 0.008(5) -0.077(6) -0.017(5) C31 0.113(6) 0.115(7) 0.099(5) -0.056(5) 0.011(5) 0.015(5) C29 0.109(6) 0.057(4) 0.158(8) -0.010(4) -0.014(6) -0.002(4) C79 0.145(8) 0.092(5) 0.172(9) -0.025(5) -0.099(7) -0.014(5) C20 0.077(5) 0.121(6) 0.131(7) -0.020(5) -0.034(4) -0.024(4) C71 0.134(7) 0.093(5) 0.097(5) -0.022(4) 0.029(5) 0.015(5) C4 0.177(10) 0.084(5) 0.096(6) 0.015(4) 0.033(6) -0.035(6) C69 0.091(5) 0.117(7) 0.139(8) 0.008(6) -0.014(5) 0.037(5) C5 0.198(11) 0.127(8) 0.102(6) 0.050(6) -0.049(7) -0.054(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 I3 Cu1 2.6903(7) . ? I3 Cu4 2.6934(7) . ? I3 Cu3 2.6976(6) . ? I2 Cu2 2.6494(7) . ? I2 Cu4 2.6628(7) . ? I2 Cu1 2.6778(7) . ? I4 Cu4 2.6848(6) . ? I4 Cu3 2.6850(6) . ? I4 Cu2 2.7087(7) . ? I1 Cu2 2.6808(7) . ? I1 Cu1 2.6926(7) . ? I1 Cu3 2.7072(7) . ? Cu4 P4 2.2523(12) . ? Cu4 Cu1 2.9955(8) . ? Cu1 P1 2.2523(12) . ? Cu1 Cu2 3.0278(8) . ? Cu2 P2 2.2474(12) . ? Cu3 P3 2.2519(12) . ? P3 C53 1.819(4) . ? P3 C47 1.846(5) . ? P3 C41 1.848(4) . ? P2 C33 1.819(4) . ? P2 C27 1.822(5) . ? P2 C21 1.823(5) . ? P4 C73 1.812(5) . ? P4 C61 1.839(5) . ? P4 C67 1.843(5) . ? P1 C13 1.816(5) . ? P1 C7 1.828(5) . ? P1 C1 1.835(5) . ? C41 C46 1.365(6) . ? C41 C42 1.389(7) . ? C58 C53 1.378(6) . ? C58 C57 1.385(6) . ? C13 C18 1.384(6) . ? C13 C14 1.386(7) . ? C73 C78 1.378(7) . ? C73 C74 1.405(6) . ? C47 C48 1.376(7) . ? C47 C52 1.386(7) . ? C33 C38 1.377(6) . ? C33 C34 1.393(6) . ? C56 N3 1.375(6) . ? C56 C55 1.395(6) . ? C56 C57 1.404(6) . ? C53 C54 1.401(6) . ? C21 C22 1.366(8) . ? C21 C26 1.373(8) . ? C67 C68 1.369(8) . ? C67 C72 1.394(8) . ? C61 C66 1.356(7) . ? C61 C62 1.370(8) . ? C48 C49 1.394(7) . ? C36 N2 1.380(6) . ? C36 C37 1.398(6) . ? C36 C35 1.406(7) . ? C8 C7 1.377(8) . ? C8 C9 1.378(8) . ? C55 C54 1.379(6) . ? C37 C38 1.392(6) . ? C7 C12 1.392(7) . ? C18 C17 1.378(8) . ? C27 C28 1.373(8) . ? C27 C32 1.379(8) . ? C46 C45 1.387(7) . ? C1 C6 1.351(9) . ? C1 C2 1.381(8) . ? C17 C16 1.397(8) . ? C42 C43 1.375(7) . ? C35 C34 1.365(6) . ? C16 N1 1.373(7) . ? C16 C15 1.402(7) . ? C78 C77 1.380(7) . ? C32 C31 1.382(10) . ? C74 C75 1.375(7) . ? C44 C45 1.340(8) . ? C44 C43 1.388(9) . ? C14 C15 1.379(8) . ? C62 C63 1.377(8) . ? C76 N4 1.371(7) . ? C76 C75 1.395(8) . ? C76 C77 1.399(7) . ? C9 C10 1.380(9) . ? C49 C50 1.383(10) . ? C52 C51 1.411(9) . ? C26 C25 1.405(10) . ? C66 C65 1.384(10) . ? C50 C51 1.343(10) . ? C22 C23 1.391(9) . ? C23 C24 1.322(11) . ? C12 C11 1.374(8) . ? C68 C69 1.396(10) . ? N3 C60 1.419(8) . ? N3 C59 1.442(7) . ? N2 C40 1.437(7) . ? N2 C39 1.451(8) . ? N1 C19 1.447(7) . ? N1 C20 1.452(9) . ? N4 C80 1.426(9) . ? N4 C79 1.439(8) . ? C28 C29 1.387(9) . ? C11 C10 1.364(10) . ? C64 C65 1.331(11) . ? C64 C63 1.365(11) . ? C2 C3 1.364(10) . ? C30 C31 1.338(12) . ? C30 C29 1.383(12) . ? C72 C71 1.383(10) . ? C6 C5 1.397(10) . ? C70 C71 1.360(12) . ? C70 C69 1.361(12) . ? C3 C4 1.347(13) . ? C24 C25 1.370(12) . ? C4 C5 1.368(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I3 Cu4 67.615(19) . . ? Cu1 I3 Cu3 70.904(19) . . ? Cu4 I3 Cu3 71.019(19) . . ? Cu2 I2 Cu4 70.90(2) . . ? Cu2 I2 Cu1 69.27(2) . . ? Cu4 I2 Cu1 68.24(2) . . ? Cu4 I4 Cu3 71.341(19) . . ? Cu4 I4 Cu2 69.671(19) . . ? Cu3 I4 Cu2 72.090(19) . . ? Cu2 I1 Cu1 68.594(19) . . ? Cu2 I1 Cu3 72.18(2) . . ? Cu1 I1 Cu3 70.724(19) . . ? P4 Cu4 I2 111.63(4) . . ? P4 Cu4 I4 104.35(4) . . ? I2 Cu4 I4 106.40(2) . . ? P4 Cu4 I3 118.35(4) . . ? I2 Cu4 I3 109.31(2) . . ? I4 Cu4 I3 105.87(2) . . ? P4 Cu4 Cu1 152.26(4) . . ? I2 Cu4 Cu1 56.120(18) . . ? I4 Cu4 Cu1 103.15(2) . . ? I3 Cu4 Cu1 56.144(18) . . ? P1 Cu1 I2 110.80(4) . . ? P1 Cu1 I3 111.14(4) . . ? I2 Cu1 I3 108.95(2) . . ? P1 Cu1 I1 112.14(4) . . ? I2 Cu1 I1 107.50(2) . . ? I3 Cu1 I1 106.11(2) . . ? P1 Cu1 Cu4 143.47(4) . . ? I2 Cu1 Cu4 55.645(18) . . ? I3 Cu1 Cu4 56.241(18) . . ? I1 Cu1 Cu4 104.39(2) . . ? P1 Cu1 Cu2 143.51(4) . . ? I2 Cu1 Cu2 54.923(18) . . ? I3 Cu1 Cu2 105.35(2) . . ? I1 Cu1 Cu2 55.518(17) . . ? Cu4 Cu1 Cu2 61.52(2) . . ? P2 Cu2 I2 116.89(4) . . ? P2 Cu2 I1 107.81(4) . . ? I2 Cu2 I1 108.68(2) . . ? P2 Cu2 I4 111.72(4) . . ? I2 Cu2 I4 106.10(2) . . ? I1 Cu2 I4 104.98(2) . . ? P2 Cu2 Cu1 146.04(4) . . ? I2 Cu2 Cu1 55.807(18) . . ? I1 Cu2 Cu1 55.888(18) . . ? I4 Cu2 Cu1 101.73(2) . . ? P3 Cu3 I4 113.30(3) . . ? P3 Cu3 I3 113.73(3) . . ? I4 Cu3 I3 105.74(2) . . ? P3 Cu3 I1 112.88(4) . . ? I4 Cu3 I1 104.90(2) . . ? I3 Cu3 I1 105.50(2) . . ? C53 P3 C47 102.6(2) . . ? C53 P3 C41 103.64(18) . . ? C47 P3 C41 103.3(2) . . ? C53 P3 Cu3 114.41(14) . . ? C47 P3 Cu3 114.71(14) . . ? C41 P3 Cu3 116.45(14) . . ? C33 P2 C27 105.4(2) . . ? C33 P2 C21 101.5(2) . . ? C27 P2 C21 103.8(2) . . ? C33 P2 Cu2 115.68(15) . . ? C27 P2 Cu2 112.80(17) . . ? C21 P2 Cu2 116.20(15) . . ? C73 P4 C61 106.2(2) . . ? C73 P4 C67 104.6(2) . . ? C61 P4 C67 102.6(2) . . ? C73 P4 Cu4 115.38(15) . . ? C61 P4 Cu4 115.16(17) . . ? C67 P4 Cu4 111.73(16) . . ? C13 P1 C7 103.6(2) . . ? C13 P1 C1 104.6(2) . . ? C7 P1 C1 103.1(2) . . ? C13 P1 Cu1 114.05(15) . . ? C7 P1 Cu1 117.11(17) . . ? C1 P1 Cu1 112.92(16) . . ? C46 C41 C42 118.1(4) . . ? C46 C41 P3 124.0(4) . . ? C42 C41 P3 117.8(3) . . ? C53 C58 C57 122.0(4) . . ? C18 C13 C14 116.3(5) . . ? C18 C13 P1 125.2(4) . . ? C14 C13 P1 118.5(4) . . ? C78 C73 C74 116.3(5) . . ? C78 C73 P4 119.6(3) . . ? C74 C73 P4 124.1(4) . . ? C48 C47 C52 118.8(5) . . ? C48 C47 P3 123.3(4) . . ? C52 C47 P3 117.8(4) . . ? C38 C33 C34 117.0(4) . . ? C38 C33 P2 119.9(3) . . ? C34 C33 P2 123.1(3) . . ? N3 C56 C55 120.9(4) . . ? N3 C56 C57 122.0(4) . . ? C55 C56 C57 117.1(4) . . ? C58 C53 C54 117.4(4) . . ? C58 C53 P3 124.9(3) . . ? C54 C53 P3 117.7(3) . . ? C58 C57 C56 120.8(4) . . ? C22 C21 C26 116.6(5) . . ? C22 C21 P2 118.5(4) . . ? C26 C21 P2 124.7(4) . . ? C68 C67 C72 119.5(6) . . ? C68 C67 P4 120.3(5) . . ? C72 C67 P4 120.1(5) . . ? C66 C61 C62 116.9(6) . . ? C66 C61 P4 124.6(5) . . ? C62 C61 P4 118.4(4) . . ? C47 C48 C49 121.7(6) . . ? N2 C36 C37 121.7(4) . . ? N2 C36 C35 121.0(4) . . ? C37 C36 C35 117.3(4) . . ? C7 C8 C9 120.9(5) . . ? C54 C55 C56 121.5(4) . . ? C38 C37 C36 120.4(4) . . ? C55 C54 C53 121.1(4) . . ? C8 C7 C12 118.2(5) . . ? C8 C7 P1 118.3(4) . . ? C12 C7 P1 123.5(4) . . ? C17 C18 C13 122.0(5) . . ? C28 C27 C32 118.3(5) . . ? C28 C27 P2 119.0(4) . . ? C32 C27 P2 122.5(5) . . ? C41 C46 C45 121.5(5) . . ? C6 C1 C2 118.8(6) . . ? C6 C1 P1 122.5(5) . . ? C2 C1 P1 118.6(5) . . ? C33 C38 C37 122.1(4) . . ? C18 C17 C16 121.6(4) . . ? C43 C42 C41 120.3(5) . . ? C34 C35 C36 120.9(4) . . ? N1 C16 C17 122.4(5) . . ? N1 C16 C15 121.1(6) . . ? C17 C16 C15 116.4(5) . . ? C35 C34 C33 122.3(4) . . ? C73 C78 C77 122.2(5) . . ? C27 C32 C31 120.1(7) . . ? C75 C74 C73 121.8(5) . . ? C45 C44 C43 120.0(5) . . ? C15 C14 C13 122.6(5) . . ? C61 C62 C63 121.7(7) . . ? N4 C76 C75 121.5(5) . . ? N4 C76 C77 122.3(5) . . ? C75 C76 C77 116.1(5) . . ? C44 C45 C46 120.0(5) . . ? C10 C9 C8 120.0(6) . . ? C78 C77 C76 121.7(5) . . ? C74 C75 C76 121.8(5) . . ? C50 C49 C48 118.7(6) . . ? C14 C15 C16 120.8(6) . . ? C47 C52 C51 119.1(6) . . ? C21 C26 C25 121.2(7) . . ? C61 C66 C65 122.0(7) . . ? C42 C43 C44 120.0(6) . . ? C51 C50 C49 120.5(6) . . ? C21 C22 C23 121.7(6) . . ? C24 C23 C22 121.6(7) . . ? C11 C12 C7 120.9(6) . . ? C67 C68 C69 119.0(7) . . ? C56 N3 C60 120.6(5) . . ? C56 N3 C59 120.5(5) . . ? C60 N3 C59 117.6(5) . . ? C36 N2 C40 121.5(5) . . ? C36 N2 C39 119.7(5) . . ? C40 N2 C39 118.4(5) . . ? C16 N1 C19 120.0(6) . . ? C16 N1 C20 122.8(5) . . ? C19 N1 C20 117.2(6) . . ? C76 N4 C80 120.4(5) . . ? C76 N4 C79 121.3(6) . . ? C80 N4 C79 117.7(6) . . ? C27 C28 C29 120.4(7) . . ? C10 C11 C12 120.2(6) . . ? C11 C10 C9 119.9(6) . . ? C50 C51 C52 121.3(6) . . ? C65 C64 C63 120.2(7) . . ? C3 C2 C1 120.5(7) . . ? C31 C30 C29 118.3(7) . . ? C71 C72 C67 119.9(7) . . ? C1 C6 C5 120.3(8) . . ? C71 C70 C69 119.3(7) . . ? C4 C3 C2 121.1(8) . . ? C23 C24 C25 118.9(7) . . ? C64 C63 C62 119.3(8) . . ? C24 C25 C26 120.0(7) . . ? C64 C65 C66 119.9(7) . . ? C30 C31 C32 122.2(8) . . ? C30 C29 C28 120.7(8) . . ? C70 C71 C72 120.7(8) . . ? C3 C4 C5 119.3(8) . . ? C70 C69 C68 121.5(8) . . ? C4 C5 C6 119.9(9) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.518 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.090 _database_code_depnum_ccdc_archive 'CCDC 880627' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_1\113K #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 4(C20H20NPCuI),C2H3N _chemical_formula_sum 'C82 H83 Cu4 I4 N5 P4' _chemical_formula_weight 2024.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3088(5) _cell_length_b 15.5278(7) _cell_length_c 16.9897(8) _cell_angle_alpha 89.042(5) _cell_angle_beta 85.531(6) _cell_angle_gamma 81.924(4) _cell_volume 3986.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11564 _cell_measurement_theta_min 2.2993 _cell_measurement_theta_max 27.5126 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1996 _exptl_absorpt_coefficient_mu 2.728 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3424 _exptl_absorpt_correction_T_max 0.4083 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39819 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.51 _reflns_number_total 17716 _reflns_number_gt 17141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+23.8921P] 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 17716 _refine_ls_number_parameters 856 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1690 _refine_ls_wR_factor_gt 0.1673 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.005 _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 I3 I 0.90547(2) 0.25857(2) 0.15588(2) 0.02303(10) Uani 1 1 d . . . I2 I 0.64060(3) 0.39894(2) 0.12230(2) 0.02271(10) Uani 1 1 d . . . I4 I 0.73359(3) 0.36148(2) 0.35521(2) 0.02125(10) Uani 1 1 d . . . Cu4 Cu 0.78216(5) 0.39049(4) 0.20388(4) 0.02241(15) Uani 1 1 d . . . Cu2 Cu 0.62133(5) 0.31225(5) 0.25548(4) 0.02323(16) Uani 1 1 d . . . Cu1 Cu 0.74000(5) 0.24391(5) 0.12310(4) 0.02696(17) Uani 1 1 d . . . Cu3 Cu 0.80938(5) 0.21420(4) 0.28529(4) 0.02135(15) Uani 1 1 d . . . P3 P 0.88874(9) 0.12375(9) 0.36667(8) 0.0182(3) Uani 1 1 d . . . P2 P 0.48430(10) 0.32321(10) 0.31526(9) 0.0222(3) Uani 1 1 d . . . P4 P 0.82489(10) 0.52295(9) 0.20652(10) 0.0239(3) Uani 1 1 d . . . P1 P 0.74212(13) 0.18354(11) 0.00350(10) 0.0325(4) Uani 1 1 d . . . C53 C 0.8303(3) 0.1020(4) 0.4596(3) 0.0174(10) Uani 1 1 d . . . C54 C 0.7846(4) 0.1729(3) 0.5021(3) 0.0207(11) Uani 1 1 d . . . H54 H 0.7812 0.2293 0.4790 0.025 Uiso 1 1 calc R . . C47 C 0.9882(4) 0.1627(3) 0.3984(4) 0.0236(11) Uani 1 1 d . . . C56 C 0.7467(3) 0.0799(4) 0.6124(3) 0.0186(10) Uani 1 1 d . . . C55 C 0.7440(4) 0.1631(4) 0.5770(3) 0.0203(10) Uani 1 1 d . . . H55 H 0.7142 0.2127 0.6047 0.024 Uiso 1 1 calc R . . C41 C 0.9306(4) 0.0151(4) 0.3275(3) 0.0214(11) Uani 1 1 d . . . C58 C 0.8310(4) 0.0199(4) 0.4945(3) 0.0204(11) Uani 1 1 d . . . H58 H 0.8611 -0.0295 0.4667 0.025 Uiso 1 1 calc R . . C35 C 0.3746(4) 0.1602(4) 0.4769(4) 0.0270(12) Uani 1 1 d . . . H35 H 0.3176 0.1445 0.4907 0.032 Uiso 1 1 calc R . . C73 C 0.9142(4) 0.5323(4) 0.2695(4) 0.0258(12) Uani 1 1 d . . . C33 C 0.4684(4) 0.2443(4) 0.3937(3) 0.0229(11) Uani 1 1 d . . . C46 C 1.0156(4) -0.0250(4) 0.3337(4) 0.0274(12) Uani 1 1 d . . . H46 H 1.0556 0.0042 0.3598 0.033 Uiso 1 1 calc R . . C36 C 0.4468(4) 0.1250(4) 0.5200(3) 0.0226(11) Uani 1 1 d . . . C37 C 0.5297(4) 0.1519(4) 0.4984(3) 0.0222(11) Uani 1 1 d . . . H37 H 0.5794 0.1301 0.5266 0.027 Uiso 1 1 calc R . . C21 C 0.3943(4) 0.3101(4) 0.2541(4) 0.0281(13) Uani 1 1 d . . . C57 C 0.7892(4) 0.0081(4) 0.5685(3) 0.0220(11) Uani 1 1 d . . . H57 H 0.7892 -0.0490 0.5896 0.026 Uiso 1 1 calc R . . N2 N 0.4354(4) 0.0666(4) 0.5803(3) 0.0308(12) Uani 1 1 d . . . N3 N 0.7070(4) 0.0700(4) 0.6869(3) 0.0315(12) Uani 1 1 d . . . C77 C 1.0028(5) 0.6157(4) 0.3423(4) 0.0308(14) Uani 1 1 d . . . H77 H 1.0160 0.6708 0.3576 0.037 Uiso 1 1 calc R . . C34 C 0.3862(4) 0.2169(4) 0.4153(4) 0.0257(12) Uani 1 1 d . . . H34 H 0.3369 0.2383 0.3864 0.031 Uiso 1 1 calc R . . C48 C 1.0469(4) 0.1928(4) 0.3412(4) 0.0287(13) Uani 1 1 d . . . H48 H 1.0358 0.1912 0.2870 0.034 Uiso 1 1 calc R . . C45 C 1.0446(4) -0.1075(4) 0.3025(4) 0.0317(14) Uani 1 1 d . . . H45 H 1.1037 -0.1344 0.3074 0.038 Uiso 1 1 calc R . . C8 C 0.8445(5) 0.0322(5) 0.0470(4) 0.0398(17) Uani 1 1 d . . . H8 H 0.8233 0.0502 0.0990 0.048 Uiso 1 1 calc R . . C60 C 0.7113(5) -0.0155(4) 0.7231(4) 0.0333(14) Uani 1 1 d . . . H60A H 0.6890 -0.0553 0.6878 0.050 Uiso 1 1 calc R . . H60B H 0.6750 -0.0117 0.7734 0.050 Uiso 1 1 calc R . . H60C H 0.7728 -0.0374 0.7327 0.050 Uiso 1 1 calc R . . N4 N 1.1187(6) 0.5430(4) 0.4201(5) 0.057(2) Uani 1 1 d . . . C52 C 1.0041(4) 0.1683(4) 0.4774(4) 0.0250(12) Uani 1 1 d . . . H52 H 0.9639 0.1488 0.5169 0.030 Uiso 1 1 calc R . . C38 C 0.5394(4) 0.2097(4) 0.4365(4) 0.0243(11) Uani 1 1 d . . . H38 H 0.5960 0.2263 0.4228 0.029 Uiso 1 1 calc R . . C51 C 1.0788(4) 0.2023(4) 0.4995(4) 0.0311(14) Uani 1 1 d . . . H51 H 1.0894 0.2059 0.5536 0.037 Uiso 1 1 calc R . . C61 C 0.7357(5) 0.6072(4) 0.2443(4) 0.0334(14) Uani 1 1 d . . . C74 C 0.9596(5) 0.4575(4) 0.2991(4) 0.0342(15) Uani 1 1 d . . . H74 H 0.9439 0.4029 0.2856 0.041 Uiso 1 1 calc R . . C7 C 0.8190(5) 0.0844(4) -0.0168(4) 0.0320(14) Uani 1 1 d . . . C76 C 1.0516(5) 0.5390(4) 0.3718(4) 0.0351(15) Uani 1 1 d . . . C15 C 0.5414(6) 0.0634(5) -0.0777(4) 0.0407(18) Uani 1 1 d . . . H15 H 0.5361 0.0126 -0.1063 0.049 Uiso 1 1 calc R . . C78 C 0.9364(4) 0.6124(4) 0.2919(4) 0.0274(12) Uani 1 1 d . . . H78 H 0.9058 0.6649 0.2724 0.033 Uiso 1 1 calc R . . C16 C 0.4655(5) 0.1208(5) -0.0550(4) 0.0367(16) Uani 1 1 d . . . C68 C 0.8675(5) 0.5120(5) 0.0451(4) 0.0349(15) Uani 1 1 d . . . H68 H 0.8552 0.4540 0.0528 0.042 Uiso 1 1 calc R . . C14 C 0.6256(5) 0.0790(4) -0.0590(4) 0.0365(16) Uani 1 1 d . . . H14 H 0.6762 0.0381 -0.0737 0.044 Uiso 1 1 calc R . . C40 C 0.5080(5) 0.0311(4) 0.6250(4) 0.0321(14) Uani 1 1 d . . . H40A H 0.5610 0.0160 0.5891 0.048 Uiso 1 1 calc R . . H40B H 0.4934 -0.0212 0.6532 0.048 Uiso 1 1 calc R . . H40C H 0.5190 0.0743 0.6631 0.048 Uiso 1 1 calc R . . C42 C 0.8726(4) -0.0276(4) 0.2884(4) 0.0292(13) Uani 1 1 d . . . H42 H 0.8139 -0.0002 0.2827 0.035 Uiso 1 1 calc R . . C67 C 0.8586(4) 0.5659(4) 0.1096(4) 0.0325(14) Uani 1 1 d . . . C50 C 1.1372(4) 0.2309(4) 0.4405(5) 0.0355(16) Uani 1 1 d . . . H50 H 1.1878 0.2542 0.4548 0.043 Uiso 1 1 calc R . . C44 C 0.9861(5) -0.1499(4) 0.2644(4) 0.0289(13) Uani 1 1 d . . . H44 H 1.0049 -0.2061 0.2428 0.035 Uiso 1 1 calc R . . C27 C 0.4483(4) 0.4288(4) 0.3609(4) 0.0306(13) Uani 1 1 d . . . C49 C 1.1222(4) 0.2256(4) 0.3628(5) 0.0362(16) Uani 1 1 d . . . H49 H 1.1630 0.2441 0.3233 0.043 Uiso 1 1 calc R . . C59 C 0.6722(5) 0.1465(5) 0.7341(4) 0.0376(16) Uani 1 1 d . . . H59A H 0.7208 0.1785 0.7447 0.056 Uiso 1 1 calc R . . H59B H 0.6439 0.1283 0.7842 0.056 Uiso 1 1 calc R . . H59C H 0.6286 0.1841 0.7052 0.056 Uiso 1 1 calc R . . C13 C 0.6351(5) 0.1547(5) -0.0189(4) 0.0360(15) Uani 1 1 d . . . C43 C 0.9004(5) -0.1097(4) 0.2579(4) 0.0326(14) Uani 1 1 d . . . H43 H 0.8601 -0.1389 0.2322 0.039 Uiso 1 1 calc R . . C66 C 0.7250(5) 0.6275(5) 0.3244(5) 0.0380(15) Uani 1 1 d . . . H66 H 0.7655 0.5996 0.3596 0.046 Uiso 1 1 calc R . . C39 C 0.3463(5) 0.0518(6) 0.6093(5) 0.0450(19) Uani 1 1 d . . . H39A H 0.3109 0.1074 0.6245 0.067 Uiso 1 1 calc R . . H39B H 0.3497 0.0128 0.6552 0.067 Uiso 1 1 calc R . . H39C H 0.3185 0.0253 0.5675 0.067 Uiso 1 1 calc R . . C75 C 1.0277(5) 0.4600(4) 0.3482(5) 0.0362(16) Uani 1 1 d . . . H75 H 1.0588 0.4069 0.3662 0.043 Uiso 1 1 calc R . . C9 C 0.9010(5) -0.0469(5) 0.0359(5) 0.0399(16) Uani 1 1 d . . . H9 H 0.9187 -0.0819 0.0798 0.048 Uiso 1 1 calc R . . C1 C 0.7699(9) 0.2567(6) -0.0773(6) 0.0642(11) Uani 1 1 d . . . C26 C 0.3168(5) 0.3673(7) 0.2523(5) 0.050(2) Uani 1 1 d . . . H26 H 0.3092 0.4188 0.2829 0.059 Uiso 1 1 calc R . . C80 C 1.1555(6) 0.4665(5) 0.4616(6) 0.052(2) Uani 1 1 d . . . H80A H 1.1074 0.4373 0.4862 0.077 Uiso 1 1 calc R . . H80B H 1.1915 0.4833 0.5025 0.077 Uiso 1 1 calc R . . H80C H 1.1926 0.4268 0.4244 0.077 Uiso 1 1 calc R . . C22 C 0.4039(6) 0.2348(5) 0.2097(5) 0.048(2) Uani 1 1 d . . . H22 H 0.4578 0.1960 0.2084 0.057 Uiso 1 1 calc R . . C32 C 0.4165(6) 0.4373(5) 0.4387(5) 0.0454(18) Uani 1 1 d . . . H32 H 0.4115 0.3865 0.4697 0.055 Uiso 1 1 calc R . . C11 C 0.9061(6) -0.0210(5) -0.1056(5) 0.0455(19) Uani 1 1 d . . . H11 H 0.9269 -0.0392 -0.1576 0.055 Uiso 1 1 calc R . . C10 C 0.9302(5) -0.0726(5) -0.0406(5) 0.0424(18) Uani 1 1 d . . . H10 H 0.9675 -0.1265 -0.0490 0.051 Uiso 1 1 calc R . . C79 C 1.1397(7) 0.6255(5) 0.4442(6) 0.057(3) Uani 1 1 d . . . H79A H 1.1375 0.6659 0.3993 0.085 Uiso 1 1 calc R . . H79B H 1.1993 0.6176 0.4630 0.085 Uiso 1 1 calc R . . H79C H 1.0967 0.6492 0.4869 0.085 Uiso 1 1 calc R . . C62 C 0.6748(7) 0.6448(7) 0.1930(6) 0.064(3) Uani 1 1 d . . . H62 H 0.6803 0.6288 0.1389 0.077 Uiso 1 1 calc R . . C69 C 0.8939(5) 0.5389(6) -0.0320(5) 0.0470(19) Uani 1 1 d . . . H69 H 0.8976 0.5008 -0.0757 0.056 Uiso 1 1 calc R . . C72 C 0.8786(8) 0.6492(6) 0.0964(6) 0.067(3) Uani 1 1 d . . . H72 H 0.8735 0.6888 0.1391 0.080 Uiso 1 1 calc R . . C12 C 0.8509(5) 0.0577(5) -0.0932(4) 0.0400(17) Uani 1 1 d . . . H12 H 0.8348 0.0936 -0.1370 0.048 Uiso 1 1 calc R . . C2 C 0.7062(9) 0.2980(6) -0.1230(6) 0.0642(11) Uani 1 1 d . . . H2 H 0.6471 0.2855 -0.1155 0.077 Uiso 1 1 calc R . . C6 C 0.8573(9) 0.2777(6) -0.0844(6) 0.0642(11) Uani 1 1 d . . . H6 H 0.9005 0.2533 -0.0501 0.077 Uiso 1 1 calc R . . N1 N 0.3822(5) 0.1072(4) -0.0739(4) 0.0446(16) Uani 1 1 d . . . C70 C 0.9142(6) 0.6222(7) -0.0416(6) 0.058(3) Uani 1 1 d . . . H70 H 0.9337 0.6417 -0.0924 0.070 Uiso 1 1 calc R . . C20 C 0.3744(7) 0.0366(6) -0.1267(5) 0.055(2) Uani 1 1 d . . . H20A H 0.4042 0.0471 -0.1784 0.083 Uiso 1 1 calc R . . H20B H 0.3118 0.0336 -0.1325 0.083 Uiso 1 1 calc R . . H20C H 0.4021 -0.0184 -0.1048 0.083 Uiso 1 1 calc R . . C28 C 0.4610(7) 0.5041(5) 0.3184(6) 0.058(3) Uani 1 1 d . . . H28 H 0.4855 0.4997 0.2652 0.069 Uiso 1 1 calc R . . C23 C 0.3349(7) 0.2153(6) 0.1668(6) 0.059(3) Uani 1 1 d . . . H23 H 0.3401 0.1619 0.1392 0.071 Uiso 1 1 calc R . . C19 C 0.3027(7) 0.1643(7) -0.0502(8) 0.074(3) Uani 1 1 d . . . H19A H 0.2958 0.1679 0.0076 0.111 Uiso 1 1 calc R . . H19B H 0.2517 0.1417 -0.0693 0.111 Uiso 1 1 calc R . . H19C H 0.3064 0.2224 -0.0725 0.111 Uiso 1 1 calc R . . C24 C 0.2575(6) 0.2761(7) 0.1649(6) 0.056(2) Uani 1 1 d . . . H24 H 0.2110 0.2648 0.1345 0.067 Uiso 1 1 calc R . . C65 C 0.6550(6) 0.6885(5) 0.3528(5) 0.0479(19) Uani 1 1 d . . . H65 H 0.6472 0.7015 0.4075 0.057 Uiso 1 1 calc R . . C30 C 0.4037(7) 0.5896(6) 0.4298(6) 0.062(3) Uani 1 1 d . . . H30 H 0.3876 0.6450 0.4538 0.074 Uiso 1 1 calc R . . C4 C 0.8129(8) 0.3758(6) -0.1917(6) 0.0642(11) Uani 1 1 d . . . H4 H 0.8285 0.4154 -0.2319 0.077 Uiso 1 1 calc R . . C71 C 0.9067(8) 0.6761(7) 0.0201(6) 0.075(4) Uani 1 1 d . . . H71 H 0.9205 0.7335 0.0122 0.090 Uiso 1 1 calc R . . C31 C 0.3920(8) 0.5168(6) 0.4726(6) 0.066(3) Uani 1 1 d . . . H31 H 0.3669 0.5213 0.5255 0.079 Uiso 1 1 calc R . . C18 C 0.5567(6) 0.2074(7) 0.0074(8) 0.077(4) Uani 1 1 d . . . H18 H 0.5610 0.2565 0.0386 0.092 Uiso 1 1 calc R . . C29 C 0.4384(8) 0.5848(6) 0.3526(7) 0.067(3) Uani 1 1 d . . . H29 H 0.4467 0.6361 0.3234 0.080 Uiso 1 1 calc R . . C5 C 0.8767(9) 0.3356(6) -0.1439(6) 0.0642(11) Uani 1 1 d . . . H5 H 0.9356 0.3483 -0.1524 0.077 Uiso 1 1 calc R . . C25 C 0.2497(6) 0.3508(8) 0.2068(6) 0.063(3) Uani 1 1 d . . . H25 H 0.1979 0.3922 0.2049 0.076 Uiso 1 1 calc R . . C64 C 0.5974(7) 0.7298(6) 0.3025(7) 0.066(3) Uani 1 1 d . . . H64 H 0.5520 0.7742 0.3218 0.079 Uiso 1 1 calc R . . C17 C 0.4745(7) 0.1923(6) -0.0092(8) 0.075(4) Uani 1 1 d . . . H17 H 0.4236 0.2302 0.0104 0.090 Uiso 1 1 calc R . . C3 C 0.7284(9) 0.3582(6) -0.1806(6) 0.0642(11) Uani 1 1 d . . . H3 H 0.6842 0.3869 -0.2120 0.077 Uiso 1 1 calc R . . C63 C 0.6048(9) 0.7070(8) 0.2227(8) 0.088(5) Uani 1 1 d . . . H63 H 0.5624 0.7336 0.1886 0.106 Uiso 1 1 calc R . . I1 I 0.67397(2) 0.14245(2) 0.23469(2) 0.02223(10) Uani 1 1 d . . . C81 C 0.3834(11) 0.4402(10) 0.0499(9) 0.101(5) Uiso 1 1 d D . . H81A H 0.3979 0.4940 0.0717 0.152 Uiso 1 1 calc R . . H81B H 0.3918 0.3934 0.0892 0.152 Uiso 1 1 calc R . . H81C H 0.3216 0.4490 0.0365 0.152 Uiso 1 1 calc R . . N5 N 0.5059(19) 0.405(2) -0.0823(17) 0.240(12) Uiso 1 1 d D . . C82 C 0.446(3) 0.415(3) -0.027(2) 0.31(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I3 0.02228(19) 0.02226(18) 0.02250(19) 0.00296(13) 0.00684(14) -0.00106(14) I2 0.02483(19) 0.02522(18) 0.01881(18) 0.00289(13) -0.00332(14) -0.00553(14) I4 0.0280(2) 0.01833(17) 0.01673(17) -0.00085(12) -0.00174(14) -0.00064(13) Cu4 0.0259(4) 0.0195(3) 0.0227(3) -0.0001(3) -0.0011(3) -0.0065(3) Cu2 0.0227(4) 0.0238(3) 0.0216(3) 0.0010(3) 0.0046(3) -0.0014(3) Cu1 0.0315(4) 0.0279(4) 0.0213(4) -0.0056(3) -0.0001(3) -0.0035(3) Cu3 0.0220(3) 0.0202(3) 0.0210(3) 0.0028(3) 0.0001(3) -0.0014(3) P3 0.0176(6) 0.0173(6) 0.0192(6) 0.0019(5) 0.0009(5) -0.0020(5) P2 0.0197(7) 0.0258(7) 0.0195(7) 0.0043(5) 0.0027(5) 0.0000(5) P4 0.0250(7) 0.0165(6) 0.0312(8) 0.0031(5) -0.0067(6) -0.0041(5) P1 0.0432(10) 0.0311(8) 0.0216(8) -0.0100(6) -0.0019(7) 0.0015(7) C53 0.014(2) 0.023(3) 0.015(2) 0.0016(19) 0.0004(18) -0.0034(19) C54 0.024(3) 0.015(2) 0.022(3) 0.005(2) -0.002(2) 0.000(2) C47 0.024(3) 0.012(2) 0.035(3) 0.005(2) -0.005(2) -0.002(2) C56 0.014(2) 0.021(3) 0.021(3) 0.003(2) -0.003(2) -0.0014(19) C55 0.018(3) 0.023(3) 0.020(3) 0.001(2) -0.001(2) -0.004(2) C41 0.021(3) 0.017(2) 0.024(3) 0.000(2) 0.002(2) -0.001(2) C58 0.021(3) 0.021(3) 0.020(3) 0.001(2) -0.001(2) -0.005(2) C35 0.019(3) 0.037(3) 0.025(3) 0.002(2) 0.000(2) -0.007(2) C73 0.030(3) 0.019(3) 0.030(3) 0.000(2) -0.006(2) -0.009(2) C33 0.022(3) 0.028(3) 0.018(3) 0.005(2) -0.001(2) -0.001(2) C46 0.025(3) 0.027(3) 0.031(3) -0.002(2) -0.002(2) -0.001(2) C36 0.021(3) 0.027(3) 0.020(3) 0.005(2) -0.001(2) -0.005(2) C37 0.020(3) 0.026(3) 0.021(3) 0.003(2) -0.004(2) -0.006(2) C21 0.024(3) 0.039(3) 0.023(3) 0.010(2) -0.001(2) -0.010(3) C57 0.022(3) 0.021(3) 0.024(3) 0.005(2) -0.003(2) -0.007(2) N2 0.027(3) 0.033(3) 0.035(3) 0.016(2) -0.007(2) -0.011(2) N3 0.036(3) 0.030(3) 0.026(3) 0.005(2) 0.007(2) -0.003(2) C77 0.038(4) 0.018(3) 0.039(4) 0.001(2) -0.015(3) -0.007(2) C34 0.014(3) 0.035(3) 0.027(3) 0.008(2) -0.003(2) -0.003(2) C48 0.024(3) 0.022(3) 0.041(4) 0.009(2) -0.002(3) -0.005(2) C45 0.023(3) 0.030(3) 0.039(4) -0.005(3) 0.001(3) 0.007(2) C8 0.047(4) 0.033(4) 0.035(4) -0.007(3) 0.017(3) -0.001(3) C60 0.038(4) 0.032(3) 0.029(3) 0.009(3) 0.001(3) -0.006(3) N4 0.073(5) 0.025(3) 0.082(5) 0.001(3) -0.055(5) -0.010(3) C52 0.019(3) 0.022(3) 0.034(3) -0.001(2) -0.002(2) -0.003(2) C38 0.021(3) 0.027(3) 0.024(3) 0.004(2) -0.001(2) -0.002(2) C51 0.023(3) 0.025(3) 0.046(4) -0.007(3) -0.011(3) 0.001(2) C61 0.032(3) 0.028(3) 0.040(4) -0.009(3) -0.008(3) -0.003(3) C74 0.037(4) 0.022(3) 0.048(4) 0.004(3) -0.024(3) -0.011(3) C7 0.033(3) 0.030(3) 0.031(3) -0.008(3) 0.006(3) -0.002(3) C76 0.043(4) 0.023(3) 0.043(4) -0.002(3) -0.019(3) -0.008(3) C15 0.065(5) 0.035(3) 0.026(3) -0.006(3) 0.012(3) -0.025(3) C78 0.035(3) 0.021(3) 0.029(3) 0.003(2) -0.009(3) -0.009(2) C16 0.054(4) 0.034(3) 0.026(3) -0.002(3) -0.012(3) -0.015(3) C68 0.030(3) 0.034(3) 0.036(4) 0.013(3) 0.006(3) 0.004(3) C14 0.052(4) 0.025(3) 0.031(3) -0.005(3) 0.016(3) -0.008(3) C40 0.037(4) 0.031(3) 0.030(3) 0.010(3) -0.009(3) -0.009(3) C42 0.026(3) 0.022(3) 0.040(4) -0.002(2) -0.006(3) -0.004(2) C67 0.029(3) 0.029(3) 0.042(4) 0.015(3) -0.013(3) -0.010(3) C50 0.020(3) 0.020(3) 0.067(5) -0.003(3) -0.009(3) -0.001(2) C44 0.036(3) 0.024(3) 0.024(3) 0.001(2) 0.002(3) 0.002(2) C27 0.021(3) 0.035(3) 0.032(3) 0.002(3) 0.003(2) 0.004(2) C49 0.021(3) 0.028(3) 0.060(5) 0.015(3) -0.006(3) -0.006(2) C59 0.050(4) 0.033(3) 0.027(3) 0.000(3) 0.011(3) -0.003(3) C13 0.046(4) 0.034(3) 0.029(3) -0.011(3) -0.014(3) 0.000(3) C43 0.037(4) 0.020(3) 0.043(4) -0.003(3) -0.013(3) -0.005(2) C66 0.038(4) 0.033(3) 0.042(4) -0.002(3) -0.004(3) -0.002(3) C39 0.038(4) 0.059(5) 0.044(4) 0.026(4) -0.012(3) -0.027(4) C75 0.042(4) 0.016(3) 0.054(4) 0.003(3) -0.028(3) -0.005(3) C9 0.042(4) 0.027(3) 0.048(4) -0.001(3) 0.008(3) -0.002(3) C1 0.100(3) 0.0391(18) 0.047(2) 0.0016(15) 0.007(2) 0.005(2) C26 0.034(4) 0.074(6) 0.039(4) 0.009(4) -0.010(3) 0.002(4) C80 0.057(5) 0.035(4) 0.067(6) 0.008(4) -0.038(5) -0.006(4) C22 0.051(5) 0.032(4) 0.064(5) 0.004(3) -0.032(4) -0.005(3) C32 0.049(5) 0.044(4) 0.037(4) -0.002(3) 0.009(3) 0.008(3) C11 0.055(5) 0.041(4) 0.037(4) -0.015(3) 0.015(4) -0.003(4) C10 0.037(4) 0.025(3) 0.059(5) -0.006(3) 0.021(3) 0.003(3) C79 0.068(6) 0.030(4) 0.079(6) -0.007(4) -0.048(5) -0.008(4) C62 0.058(6) 0.067(6) 0.060(6) -0.021(5) -0.028(5) 0.030(5) C69 0.038(4) 0.062(5) 0.040(4) 0.023(4) 0.004(3) -0.012(4) C72 0.114(9) 0.041(4) 0.060(6) 0.029(4) -0.050(6) -0.044(5) C12 0.051(4) 0.040(4) 0.024(3) -0.007(3) 0.005(3) 0.004(3) C2 0.100(3) 0.0391(18) 0.047(2) 0.0016(15) 0.007(2) 0.005(2) C6 0.100(3) 0.0391(18) 0.047(2) 0.0016(15) 0.007(2) 0.005(2) N1 0.058(4) 0.043(4) 0.039(3) -0.013(3) -0.008(3) -0.025(3) C70 0.040(4) 0.088(7) 0.056(5) 0.043(5) -0.020(4) -0.035(5) C20 0.075(6) 0.054(5) 0.046(5) -0.017(4) 0.000(4) -0.043(5) C28 0.076(6) 0.036(4) 0.048(5) 0.007(4) 0.024(5) 0.018(4) C23 0.070(6) 0.040(4) 0.078(7) 0.011(4) -0.042(5) -0.024(4) C19 0.069(7) 0.058(6) 0.101(9) -0.021(6) -0.055(6) -0.003(5) C24 0.044(5) 0.082(7) 0.047(5) 0.026(5) -0.024(4) -0.021(5) C65 0.046(5) 0.045(4) 0.052(5) -0.016(4) -0.003(4) -0.002(4) C30 0.066(6) 0.038(4) 0.073(7) -0.019(4) 0.003(5) 0.017(4) C4 0.100(3) 0.0391(18) 0.047(2) 0.0016(15) 0.007(2) 0.005(2) C71 0.105(9) 0.070(6) 0.072(7) 0.054(6) -0.048(6) -0.068(7) C31 0.082(7) 0.050(5) 0.056(6) -0.016(4) 0.019(5) 0.014(5) C18 0.048(5) 0.060(6) 0.122(10) -0.067(6) -0.043(6) 0.024(4) C29 0.089(8) 0.033(4) 0.071(7) 0.001(4) 0.004(6) 0.009(5) C5 0.100(3) 0.0391(18) 0.047(2) 0.0016(15) 0.007(2) 0.005(2) C25 0.033(4) 0.098(8) 0.054(5) 0.017(5) -0.012(4) 0.005(5) C64 0.058(6) 0.051(5) 0.082(7) -0.031(5) -0.007(5) 0.019(4) C17 0.064(6) 0.051(5) 0.113(9) -0.047(6) -0.049(6) 0.012(5) C3 0.100(3) 0.0391(18) 0.047(2) 0.0016(15) 0.007(2) 0.005(2) C63 0.085(8) 0.077(8) 0.092(9) -0.035(7) -0.045(7) 0.051(7) I1 0.02548(19) 0.01735(17) 0.02424(19) -0.00089(13) -0.00259(14) -0.00386(13) _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 I3 Cu4 2.6747(8) . ? I3 Cu1 2.6767(9) . ? I3 Cu3 2.6837(8) . ? I2 Cu2 2.6314(8) . ? I2 Cu4 2.6489(8) . ? I2 Cu1 2.6615(9) . ? I4 Cu3 2.6678(8) . ? I4 Cu4 2.6689(8) . ? I4 Cu2 2.6972(8) . ? Cu4 P4 2.2464(16) . ? Cu4 Cu1 2.8523(10) . ? Cu4 Cu2 2.9623(10) . ? Cu4 Cu3 3.0368(10) . ? Cu2 P2 2.2438(16) . ? Cu2 I1 2.6675(8) . ? Cu2 Cu1 2.8959(10) . ? Cu1 P1 2.2480(17) . ? Cu1 I1 2.6734(9) . ? Cu1 Cu3 3.0348(10) . ? Cu3 P3 2.2534(16) . ? Cu3 I1 2.6902(8) . ? P3 C53 1.805(5) . ? P3 C41 1.835(6) . ? P3 C47 1.836(6) . ? P2 C33 1.821(6) . ? P2 C27 1.821(7) . ? P2 C21 1.825(6) . ? P4 C73 1.823(6) . ? P4 C67 1.830(7) . ? P4 C61 1.838(7) . ? P1 C7 1.821(7) . ? P1 C13 1.827(8) . ? P1 C1 1.830(10) . ? C53 C58 1.395(8) . ? C53 C54 1.398(8) . ? C54 C55 1.389(8) . ? C47 C52 1.388(9) . ? C47 C48 1.393(9) . ? C56 N3 1.377(8) . ? C56 C57 1.403(8) . ? C56 C55 1.414(8) . ? C41 C46 1.373(8) . ? C41 C42 1.393(8) . ? C58 C57 1.387(8) . ? C35 C34 1.373(9) . ? C35 C36 1.413(8) . ? C73 C74 1.375(9) . ? C73 C78 1.402(8) . ? C33 C38 1.394(8) . ? C33 C34 1.405(8) . ? C46 C45 1.395(9) . ? C36 N2 1.375(8) . ? C36 C37 1.411(8) . ? C37 C38 1.384(8) . ? C21 C26 1.381(11) . ? C21 C22 1.386(11) . ? N2 C40 1.435(8) . ? N2 C39 1.462(9) . ? N3 C60 1.449(8) . ? N3 C59 1.457(9) . ? C77 C78 1.386(9) . ? C77 C76 1.419(9) . ? C48 C49 1.400(9) . ? C45 C44 1.388(10) . ? C8 C7 1.390(11) . ? C8 C9 1.405(10) . ? N4 C76 1.372(9) . ? N4 C79 1.437(9) . ? N4 C80 1.440(10) . ? C52 C51 1.404(8) . ? C51 C50 1.399(11) . ? C61 C62 1.388(11) . ? C61 C66 1.394(10) . ? C74 C75 1.391(9) . ? C7 C12 1.399(9) . ? C76 C75 1.402(8) . ? C15 C16 1.394(12) . ? C15 C14 1.405(12) . ? C16 N1 1.384(10) . ? C16 C17 1.395(10) . ? C68 C67 1.377(11) . ? C68 C69 1.415(10) . ? C14 C13 1.399(9) . ? C42 C43 1.382(9) . ? C67 C72 1.382(9) . ? C50 C49 1.363(11) . ? C44 C43 1.384(10) . ? C27 C32 1.374(10) . ? C27 C28 1.393(11) . ? C13 C18 1.401(11) . ? C66 C65 1.388(11) . ? C9 C10 1.388(11) . ? C1 C2 1.375(16) . ? C1 C6 1.417(17) . ? C26 C25 1.385(13) . ? C22 C23 1.398(11) . ? C32 C31 1.362(12) . ? C11 C12 1.393(11) . ? C11 C10 1.396(12) . ? C62 C63 1.407(13) . ? C69 C70 1.377(13) . ? C72 C71 1.408(14) . ? C2 C3 1.398(13) . ? C6 C5 1.384(13) . ? N1 C19 1.436(13) . ? N1 C20 1.451(9) . ? C70 C71 1.340(16) . ? C28 C29 1.379(12) . ? C23 C24 1.408(14) . ? C24 C25 1.358(16) . ? C65 C64 1.363(14) . ? C30 C31 1.359(15) . ? C30 C29 1.376(15) . ? C4 C3 1.359(17) . ? C4 C5 1.392(16) . ? C18 C17 1.362(13) . ? C64 C63 1.399(16) . ? C81 C82 1.579(18) . ? N5 C82 1.257(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 Cu4 I3 Cu1 64.42(2) . . ? Cu4 I3 Cu3 69.05(2) . . ? Cu1 I3 Cu3 68.96(2) . . ? Cu2 I2 Cu4 68.25(2) . . ? Cu2 I2 Cu1 66.34(2) . . ? Cu4 I2 Cu1 64.98(2) . . ? Cu3 I4 Cu4 69.37(2) . . ? Cu3 I4 Cu2 71.53(2) . . ? Cu4 I4 Cu2 67.01(2) . . ? P4 Cu4 I2 109.13(5) . . ? P4 Cu4 I4 102.89(5) . . ? I2 Cu4 I4 108.35(3) . . ? P4 Cu4 I3 116.94(5) . . ? I2 Cu4 I3 111.45(3) . . ? I4 Cu4 I3 107.44(3) . . ? P4 Cu4 Cu1 152.47(5) . . ? I2 Cu4 Cu1 57.72(2) . . ? I4 Cu4 Cu1 104.31(3) . . ? I3 Cu4 Cu1 57.82(2) . . ? P4 Cu4 Cu2 136.51(5) . . ? I2 Cu4 Cu2 55.60(2) . . ? I4 Cu4 Cu2 56.95(2) . . ? I3 Cu4 Cu2 106.24(3) . . ? Cu1 Cu4 Cu2 59.70(3) . . ? P4 Cu4 Cu3 141.10(5) . . ? I2 Cu4 Cu3 108.48(3) . . ? I4 Cu4 Cu3 55.30(2) . . ? I3 Cu4 Cu3 55.62(2) . . ? Cu1 Cu4 Cu3 61.94(2) . . ? Cu2 Cu4 Cu3 63.01(2) . . ? P2 Cu2 I2 116.86(5) . . ? P2 Cu2 I1 105.76(5) . . ? I2 Cu2 I1 111.11(3) . . ? P2 Cu2 I4 109.91(5) . . ? I2 Cu2 I4 108.02(3) . . ? I1 Cu2 I4 104.48(3) . . ? P2 Cu2 Cu1 146.73(5) . . ? I2 Cu2 Cu1 57.33(2) . . ? I1 Cu2 Cu1 57.27(2) . . ? I4 Cu2 Cu1 102.43(3) . . ? P2 Cu2 Cu4 150.61(5) . . ? I2 Cu2 Cu4 56.16(2) . . ? I1 Cu2 Cu4 102.99(3) . . ? I4 Cu2 Cu4 56.04(2) . . ? Cu1 Cu2 Cu4 58.26(2) . . ? P1 Cu1 I2 108.59(6) . . ? P1 Cu1 I1 110.39(6) . . ? I2 Cu1 I1 109.99(3) . . ? P1 Cu1 I3 109.53(6) . . ? I2 Cu1 I3 111.00(3) . . ? I1 Cu1 I3 107.35(3) . . ? P1 Cu1 Cu4 143.79(6) . . ? I2 Cu1 Cu4 57.30(2) . . ? I1 Cu1 Cu4 105.82(3) . . ? I3 Cu1 Cu4 57.76(2) . . ? P1 Cu1 Cu2 142.40(6) . . ? I2 Cu1 Cu2 56.33(2) . . ? I1 Cu1 Cu2 57.07(2) . . ? I3 Cu1 Cu2 108.07(3) . . ? Cu4 Cu1 Cu2 62.03(3) . . ? P1 Cu1 Cu3 143.21(6) . . ? I2 Cu1 Cu3 108.20(3) . . ? I1 Cu1 Cu3 55.80(2) . . ? I3 Cu1 Cu3 55.63(2) . . ? Cu4 Cu1 Cu3 62.02(2) . . ? Cu2 Cu1 Cu3 63.79(3) . . ? P3 Cu3 I4 112.99(5) . . ? P3 Cu3 I3 113.12(5) . . ? I4 Cu3 I3 107.21(3) . . ? P3 Cu3 I1 111.62(4) . . ? I4 Cu3 I1 104.67(3) . . ? I3 Cu3 I1 106.66(3) . . ? P3 Cu3 Cu1 147.38(5) . . ? I4 Cu3 Cu1 99.58(3) . . ? I3 Cu3 Cu1 55.41(2) . . ? I1 Cu3 Cu1 55.28(2) . . ? P3 Cu3 Cu4 147.85(5) . . ? I4 Cu3 Cu4 55.33(2) . . ? I3 Cu3 Cu4 55.34(2) . . ? I1 Cu3 Cu4 100.52(3) . . ? Cu1 Cu3 Cu4 56.04(2) . . ? C53 P3 C41 103.7(3) . . ? C53 P3 C47 102.2(3) . . ? C41 P3 C47 103.4(3) . . ? C53 P3 Cu3 114.69(19) . . ? C41 P3 Cu3 115.8(2) . . ? C47 P3 Cu3 115.26(18) . . ? C33 P2 C27 104.9(3) . . ? C33 P2 C21 101.5(3) . . ? C27 P2 C21 103.1(3) . . ? C33 P2 Cu2 115.4(2) . . ? C27 P2 Cu2 112.9(2) . . ? C21 P2 Cu2 117.3(2) . . ? C73 P4 C67 106.5(3) . . ? C73 P4 C61 103.6(3) . . ? C67 P4 C61 102.9(3) . . ? C73 P4 Cu4 115.2(2) . . ? C67 P4 Cu4 114.6(2) . . ? C61 P4 Cu4 112.9(2) . . ? C7 P1 C13 104.0(3) . . ? C7 P1 C1 103.7(4) . . ? C13 P1 C1 103.9(5) . . ? C7 P1 Cu1 117.5(2) . . ? C13 P1 Cu1 113.4(2) . . ? C1 P1 Cu1 112.9(3) . . ? C58 C53 C54 117.3(5) . . ? C58 C53 P3 124.9(4) . . ? C54 C53 P3 117.8(4) . . ? C55 C54 C53 121.8(5) . . ? C52 C47 C48 118.9(6) . . ? C52 C47 P3 122.5(5) . . ? C48 C47 P3 118.5(5) . . ? N3 C56 C57 121.5(5) . . ? N3 C56 C55 120.6(5) . . ? C57 C56 C55 117.9(5) . . ? C54 C55 C56 120.4(5) . . ? C46 C41 C42 118.9(5) . . ? C46 C41 P3 123.5(5) . . ? C42 C41 P3 117.5(5) . . ? C57 C58 C53 122.1(5) . . ? C34 C35 C36 120.6(5) . . ? C74 C73 C78 118.3(6) . . ? C74 C73 P4 118.7(4) . . ? C78 C73 P4 123.0(5) . . ? C38 C33 C34 117.0(5) . . ? C38 C33 P2 120.0(5) . . ? C34 C33 P2 123.0(4) . . ? C41 C46 C45 121.5(6) . . ? N2 C36 C37 122.0(5) . . ? N2 C36 C35 120.4(5) . . ? C37 C36 C35 117.6(5) . . ? C38 C37 C36 120.6(5) . . ? C26 C21 C22 118.7(7) . . ? C26 C21 P2 124.6(6) . . ? C22 C21 P2 116.7(5) . . ? C58 C57 C56 120.4(5) . . ? C36 N2 C40 120.9(5) . . ? C36 N2 C39 120.0(5) . . ? C40 N2 C39 118.2(5) . . ? C56 N3 C60 120.1(5) . . ? C56 N3 C59 119.9(5) . . ? C60 N3 C59 119.4(5) . . ? C78 C77 C76 121.7(6) . . ? C35 C34 C33 122.1(6) . . ? C47 C48 C49 120.5(7) . . ? C44 C45 C46 119.1(6) . . ? C7 C8 C9 121.2(7) . . ? C76 N4 C79 120.7(6) . . ? C76 N4 C80 120.2(6) . . ? C79 N4 C80 117.6(6) . . ? C47 C52 C51 120.8(6) . . ? C37 C38 C33 122.0(6) . . ? C50 C51 C52 118.9(7) . . ? C62 C61 C66 120.6(7) . . ? C62 C61 P4 118.7(6) . . ? C66 C61 P4 120.5(6) . . ? C73 C74 C75 121.7(6) . . ? C8 C7 C12 119.1(6) . . ? C8 C7 P1 117.8(5) . . ? C12 C7 P1 123.1(6) . . ? N4 C76 C75 122.5(6) . . ? N4 C76 C77 121.2(6) . . ? C75 C76 C77 116.3(6) . . ? C16 C15 C14 121.5(6) . . ? C77 C78 C73 120.5(6) . . ? N1 C16 C15 122.3(6) . . ? N1 C16 C17 119.5(8) . . ? C15 C16 C17 118.1(8) . . ? C67 C68 C69 123.1(7) . . ? C13 C14 C15 120.1(7) . . ? C43 C42 C41 120.1(6) . . ? C68 C67 C72 116.7(7) . . ? C68 C67 P4 118.9(5) . . ? C72 C67 P4 124.4(7) . . ? C49 C50 C51 120.7(6) . . ? C43 C44 C45 119.6(6) . . ? C32 C27 C28 118.1(7) . . ? C32 C27 P2 122.4(6) . . ? C28 C27 P2 119.3(5) . . ? C50 C49 C48 120.1(7) . . ? C14 C13 C18 116.3(7) . . ? C14 C13 P1 123.4(6) . . ? C18 C13 P1 120.2(5) . . ? C42 C43 C44 120.7(6) . . ? C65 C66 C61 119.9(7) . . ? C74 C75 C76 121.4(6) . . ? C10 C9 C8 118.5(7) . . ? C2 C1 C6 121.0(10) . . ? C2 C1 P1 121.4(10) . . ? C6 C1 P1 117.1(8) . . ? C21 C26 C25 121.2(9) . . ? C21 C22 C23 120.6(8) . . ? C31 C32 C27 121.7(8) . . ? C12 C11 C10 119.1(7) . . ? C9 C10 C11 121.4(7) . . ? C61 C62 C63 118.6(9) . . ? C70 C69 C68 117.7(9) . . ? C67 C72 C71 120.6(10) . . ? C11 C12 C7 120.7(7) . . ? C1 C2 C3 120.1(12) . . ? C5 C6 C1 116.6(11) . . ? C16 N1 C19 123.5(6) . . ? C16 N1 C20 118.9(7) . . ? C19 N1 C20 117.3(7) . . ? C71 C70 C69 120.6(8) . . ? C29 C28 C27 120.6(8) . . ? C22 C23 C24 119.1(9) . . ? C25 C24 C23 119.8(8) . . ? C64 C65 C66 120.4(8) . . ? C31 C30 C29 121.3(8) . . ? C3 C4 C5 119.6(10) . . ? C70 C71 C72 121.3(8) . . ? C30 C31 C32 119.4(9) . . ? C17 C18 C13 123.9(7) . . ? C30 C29 C28 118.8(9) . . ? C6 C5 C4 122.4(12) . . ? C24 C25 C26 120.5(9) . . ? C65 C64 C63 120.2(8) . . ? C18 C17 C16 119.6(9) . . ? C4 C3 C2 120.1(11) . . ? C64 C63 C62 120.1(9) . . ? Cu2 I1 Cu1 65.67(2) . . ? Cu2 I1 Cu3 71.64(2) . . ? Cu1 I1 Cu3 68.92(2) . . ? N5 C82 C81 168(5) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.006 _refine_diff_density_min -1.871 _refine_diff_density_rms 0.146 _database_code_depnum_ccdc_archive 'CCDC 880628' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form ###END data_1\160K #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 4(C20H20N1P1Cu1I1) _chemical_formula_sum 'C80 H80 Cu4 I4 N4 P4' _chemical_formula_weight 1983.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3491(4) _cell_length_b 15.4845(4) _cell_length_c 16.9896(4) _cell_angle_alpha 88.448(2) _cell_angle_beta 85.496(2) _cell_angle_gamma 81.231(2) _cell_volume 3977.98(17) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 23761 _cell_measurement_theta_min 2.6069 _cell_measurement_theta_max 74.0411 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2653 _exptl_crystal_size_mid 0.2031 _exptl_crystal_size_min 0.1483 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 14.487 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0519 _exptl_absorpt_correction_T_max 0.0978 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5992 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42748 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 66.60 _reflns_number_total 14036 _reflns_number_gt 12417 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _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^)+(0.0312P)^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 14036 _refine_ls_number_parameters 873 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0549 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 0.632657(12) 0.409158(11) 0.122946(11) 0.03671(5) Uani 1 1 d . . . I1 I 0.670513(11) 0.144560(11) 0.230554(11) 0.03448(5) Uani 1 1 d . . . I4 I 0.737488(12) 0.362444(11) 0.352023(10) 0.03559(5) Uani 1 1 d . . . I3 I 0.899815(11) 0.258738(11) 0.149417(10) 0.03428(5) Uani 1 1 d . . . Cu2 Cu 0.62258(3) 0.31525(3) 0.25534(3) 0.03997(10) Uani 1 1 d . . . Cu3 Cu 0.80705(3) 0.21328(3) 0.28061(2) 0.03692(9) Uani 1 1 d . . . Cu1 Cu 0.73220(3) 0.25205(3) 0.11935(3) 0.03969(10) Uani 1 1 d . . . Cu4 Cu 0.77931(3) 0.39384(3) 0.19951(3) 0.03779(10) Uani 1 1 d . . . P3 P 0.88863(5) 0.12256(4) 0.36178(4) 0.03162(14) Uani 1 1 d . . . P4 P 0.82548(5) 0.52490(5) 0.20100(4) 0.03527(15) Uani 1 1 d . . . P1 P 0.73263(5) 0.19221(5) -0.00013(4) 0.03760(16) Uani 1 1 d . . . P2 P 0.48706(5) 0.32502(5) 0.31862(4) 0.03446(15) Uani 1 1 d . . . C54 C 0.83117(19) 0.01971(18) 0.49128(17) 0.0342(6) Uani 1 1 d . . . H54 H 0.8600 -0.0303 0.4634 0.041 Uiso 1 1 calc R . . C56 C 0.74793(18) 0.08139(19) 0.60958(16) 0.0344(6) Uani 1 1 d . . . C53 C 0.83121(18) 0.10238(18) 0.45695(16) 0.0320(6) Uani 1 1 d . . . C58 C 0.78812(18) 0.17412(18) 0.49909(17) 0.0334(6) Uani 1 1 d . . . H58 H 0.7862 0.2309 0.4761 0.040 Uiso 1 1 calc R . . C13 C 0.6272(2) 0.1609(2) -0.01955(17) 0.0397(7) Uani 1 1 d . . . C2 C 0.8409(2) 0.0408(2) 0.0418(2) 0.0433(7) Uani 1 1 d . . . H2 H 0.8216 0.0582 0.0943 0.052 Uiso 1 1 calc R . . C57 C 0.74791(19) 0.16451(19) 0.57398(17) 0.0364(6) Uani 1 1 d . . . H57 H 0.7198 0.2149 0.6018 0.044 Uiso 1 1 calc R . . N3 N 0.70792(19) 0.07214(17) 0.68409(16) 0.0456(6) Uani 1 1 d . . . C34 C 0.54155(19) 0.20741(19) 0.43884(17) 0.0376(6) Uani 1 1 d . . . H34 H 0.5987 0.2220 0.4248 0.045 Uiso 1 1 calc R . . C62 C 0.8630(2) 0.5135(2) 0.03935(19) 0.0481(8) Uani 1 1 d . . . H62 H 0.8431 0.4584 0.0465 0.058 Uiso 1 1 calc R . . N1 N 0.3754(2) 0.1093(2) -0.06863(19) 0.0560(7) Uani 1 1 d . . . C21 C 0.3980(2) 0.3131(2) 0.25620(17) 0.0394(6) Uani 1 1 d . . . C47 C 0.93042(19) 0.01263(18) 0.32415(17) 0.0349(6) Uani 1 1 d . . . C33 C 0.47100(19) 0.24482(19) 0.39615(17) 0.0358(6) Uani 1 1 d . . . C55 C 0.78955(19) 0.00934(19) 0.56568(18) 0.0373(6) Uani 1 1 d . . . H55 H 0.7893 -0.0479 0.5873 0.045 Uiso 1 1 calc R . . C61 C 0.86206(19) 0.56609(19) 0.10384(18) 0.0390(6) Uani 1 1 d . . . C73 C 0.9128(2) 0.53349(19) 0.26521(18) 0.0386(6) Uani 1 1 d . . . C18 C 0.6174(2) 0.0880(2) -0.06188(18) 0.0425(7) Uani 1 1 d . . . H18 H 0.6685 0.0493 -0.0804 0.051 Uiso 1 1 calc R . . C7 C 0.7572(2) 0.2663(2) -0.08204(18) 0.0421(7) Uani 1 1 d . . . C41 C 0.98861(18) 0.16234(18) 0.38979(18) 0.0358(6) Uani 1 1 d . . . C27 C 0.45166(19) 0.4303(2) 0.36606(18) 0.0393(6) Uani 1 1 d . . . C36 C 0.4471(2) 0.1254(2) 0.52336(18) 0.0397(7) Uani 1 1 d . . . C17 C 0.5352(2) 0.0702(2) -0.07770(19) 0.0455(7) Uani 1 1 d . . . H17 H 0.5312 0.0199 -0.1072 0.055 Uiso 1 1 calc R . . C37 C 0.37625(19) 0.1629(2) 0.47932(18) 0.0405(7) Uani 1 1 d . . . H37 H 0.3190 0.1481 0.4923 0.049 Uiso 1 1 calc R . . C75 C 0.9975(2) 0.61567(19) 0.3425(2) 0.0465(8) Uani 1 1 d . . . H75 H 1.0084 0.6707 0.3596 0.056 Uiso 1 1 calc R . . C78 C 0.9630(2) 0.4575(2) 0.2924(2) 0.0449(7) Uani 1 1 d . . . H78 H 0.9517 0.4026 0.2752 0.054 Uiso 1 1 calc R . . C23 C 0.3332(2) 0.2188(2) 0.1740(2) 0.0533(8) Uani 1 1 d . . . H23 H 0.3351 0.1632 0.1511 0.064 Uiso 1 1 calc R . . C16 C 0.4573(2) 0.1245(2) -0.05126(18) 0.0432(7) Uani 1 1 d . . . C45 C 1.0804(2) 0.2045(2) 0.4869(2) 0.0526(9) Uani 1 1 d . . . H45 H 1.0915 0.2100 0.5406 0.063 Uiso 1 1 calc R . . C35 C 0.5306(2) 0.14979(19) 0.50092(18) 0.0383(6) Uani 1 1 d . . . H35 H 0.5801 0.1261 0.5291 0.046 Uiso 1 1 calc R . . C38 C 0.3888(2) 0.2202(2) 0.41798(18) 0.0409(7) Uani 1 1 d . . . H38 H 0.3396 0.2440 0.3894 0.049 Uiso 1 1 calc R . . C1 C 0.8123(2) 0.0939(2) -0.02134(19) 0.0413(7) Uani 1 1 d . . . C46 C 1.0064(2) 0.1701(2) 0.4680(2) 0.0434(7) Uani 1 1 d . . . H46 H 0.9675 0.1516 0.5091 0.052 Uiso 1 1 calc R . . C77 C 1.0285(2) 0.4591(2) 0.3433(2) 0.0495(8) Uani 1 1 d . . . H77 H 1.0606 0.4057 0.3610 0.059 Uiso 1 1 calc R . . C67 C 0.7363(2) 0.61076(19) 0.2367(2) 0.0425(7) Uani 1 1 d . . . C52 C 1.0138(2) -0.0309(2) 0.33698(19) 0.0425(7) Uani 1 1 d . . . H52 H 1.0520 -0.0041 0.3667 0.051 Uiso 1 1 calc R . . C6 C 0.8433(2) 0.0683(2) -0.0976(2) 0.0517(8) Uani 1 1 d . . . H6 H 0.8255 0.1046 -0.1412 0.062 Uiso 1 1 calc R . . C50 C 0.9874(2) -0.1536(2) 0.2640(2) 0.0479(8) Uani 1 1 d . . . H50 H 1.0069 -0.2102 0.2431 0.058 Uiso 1 1 calc R . . C22 C 0.4001(2) 0.2333(2) 0.2200(2) 0.0482(8) Uani 1 1 d . . . H22 H 0.4482 0.1880 0.2270 0.058 Uiso 1 1 calc R . . N4 N 1.1137(2) 0.5416(2) 0.4192(2) 0.0706(10) Uani 1 1 d . . . C76 C 1.0485(2) 0.5388(2) 0.3695(2) 0.0488(8) Uani 1 1 d . . . C60 C 0.6729(3) 0.1488(2) 0.7296(2) 0.0543(9) Uani 1 1 d . . . H60A H 0.7210 0.1813 0.7391 0.082 Uiso 1 1 calc R . . H60B H 0.6454 0.1311 0.7803 0.082 Uiso 1 1 calc R . . H60C H 0.6287 0.1861 0.7004 0.082 Uiso 1 1 calc R . . C8 C 0.8423(2) 0.2870(2) -0.0945(2) 0.0531(8) Uani 1 1 d . . . H8 H 0.8868 0.2612 -0.0617 0.064 Uiso 1 1 calc R . . C68 C 0.6782(2) 0.6543(2) 0.1849(2) 0.0541(8) Uani 1 1 d . . . H68 H 0.6860 0.6411 0.1303 0.065 Uiso 1 1 calc R . . C51 C 1.0419(2) -0.1141(2) 0.3063(2) 0.0492(8) Uani 1 1 d . . . H51 H 1.0995 -0.1435 0.3150 0.059 Uiso 1 1 calc R . . C44 C 1.1377(2) 0.2306(2) 0.4280(3) 0.0560(10) Uani 1 1 d . . . H44 H 1.1883 0.2541 0.4410 0.067 Uiso 1 1 calc R . . C64 C 0.9210(2) 0.6191(3) -0.0462(2) 0.0549(9) Uani 1 1 d . . . H64 H 0.9416 0.6371 -0.0973 0.066 Uiso 1 1 calc R . . C42 C 1.0470(2) 0.1895(2) 0.3306(2) 0.0479(8) Uani 1 1 d . . . H42 H 1.0359 0.1853 0.2768 0.057 Uiso 1 1 calc R . . C3 C 0.8974(2) -0.0373(2) 0.0289(2) 0.0522(8) Uani 1 1 d . . . H3 H 0.9163 -0.0731 0.0725 0.063 Uiso 1 1 calc R . . C66 C 0.8910(2) 0.6468(2) 0.0921(2) 0.0508(8) Uani 1 1 d . . . H66 H 0.8907 0.6841 0.1356 0.061 Uiso 1 1 calc R . . C65 C 0.9201(3) 0.6728(2) 0.0171(2) 0.0584(9) Uani 1 1 d . . . H65 H 0.9395 0.7280 0.0095 0.070 Uiso 1 1 calc R . . C39 C 0.5070(2) 0.0272(2) 0.6289(2) 0.0506(8) Uani 1 1 d . . . H39A H 0.5595 0.0096 0.5929 0.076 Uiso 1 1 calc R . . H39B H 0.4903 -0.0244 0.6574 0.076 Uiso 1 1 calc R . . H39C H 0.5202 0.0691 0.6668 0.076 Uiso 1 1 calc R . . C14 C 0.5503(2) 0.2123(2) 0.0099(2) 0.0505(8) Uani 1 1 d . . . H14 H 0.5549 0.2605 0.0420 0.061 Uiso 1 1 calc R . . C15 C 0.4672(2) 0.1965(2) -0.0057(2) 0.0512(8) Uani 1 1 d . . . H15 H 0.4163 0.2344 0.0146 0.061 Uiso 1 1 calc R . . C48 C 0.8753(2) -0.0280(2) 0.2811(2) 0.0479(8) Uani 1 1 d . . . H48 H 0.8179 0.0013 0.2718 0.057 Uiso 1 1 calc R . . C9 C 0.8628(3) 0.3446(2) -0.1539(2) 0.0616(10) Uani 1 1 d . . . H9 H 0.9213 0.3579 -0.1619 0.074 Uiso 1 1 calc R . . C74 C 0.9321(2) 0.6127(2) 0.2917(2) 0.0439(7) Uani 1 1 d . . . H74 H 0.8994 0.6659 0.2743 0.053 Uiso 1 1 calc R . . C59 C 0.7126(3) -0.0130(2) 0.7220(2) 0.0535(9) Uani 1 1 d . . . H59A H 0.6887 -0.0528 0.6883 0.080 Uiso 1 1 calc R . . H59B H 0.6779 -0.0080 0.7730 0.080 Uiso 1 1 calc R . . H59C H 0.7743 -0.0361 0.7302 0.080 Uiso 1 1 calc R . . C28 C 0.4704(2) 0.5054(2) 0.3270(2) 0.0528(8) Uani 1 1 d . . . H28 H 0.5000 0.5018 0.2757 0.063 Uiso 1 1 calc R . . C43 C 1.1216(2) 0.2227(2) 0.3504(3) 0.0559(9) Uani 1 1 d . . . H43 H 1.1618 0.2401 0.3098 0.067 Uiso 1 1 calc R . . C12 C 0.6926(3) 0.3065(2) -0.1292(2) 0.0560(9) Uani 1 1 d . . . H12 H 0.6338 0.2941 -0.1211 0.067 Uiso 1 1 calc R . . C4 C 0.9263(2) -0.0633(2) -0.0475(3) 0.0595(10) Uani 1 1 d . . . H4 H 0.9638 -0.1174 -0.0565 0.071 Uiso 1 1 calc R . . C10 C 0.7987(3) 0.3828(2) -0.2018(2) 0.0658(11) Uani 1 1 d . . . H10 H 0.8131 0.4212 -0.2437 0.079 Uiso 1 1 calc R . . C20 C 0.2951(2) 0.1617(3) -0.0387(3) 0.0637(10) Uani 1 1 d . . . H20A H 0.2884 0.1549 0.0189 0.096 Uiso 1 1 calc R . . H20B H 0.2448 0.1427 -0.0618 0.096 Uiso 1 1 calc R . . H20C H 0.2973 0.2232 -0.0526 0.096 Uiso 1 1 calc R . . C72 C 0.7213(2) 0.6284(2) 0.3169(2) 0.0541(8) Uani 1 1 d . . . H72 H 0.7589 0.5974 0.3533 0.065 Uiso 1 1 calc R . . C5 C 0.8999(3) -0.0097(3) -0.1107(2) 0.0602(10) Uani 1 1 d . . . H5 H 0.9206 -0.0264 -0.1630 0.072 Uiso 1 1 calc R . . C70 C 0.5968(3) 0.7358(3) 0.2923(3) 0.0705(12) Uani 1 1 d . . . H70 H 0.5505 0.7799 0.3111 0.085 Uiso 1 1 calc R . . C49 C 0.9034(3) -0.1107(2) 0.2517(2) 0.0542(9) Uani 1 1 d . . . H49 H 0.8649 -0.1383 0.2230 0.065 Uiso 1 1 calc R . . C63 C 0.8922(3) 0.5394(3) -0.0357(2) 0.0572(9) Uani 1 1 d . . . H63 H 0.8923 0.5024 -0.0794 0.069 Uiso 1 1 calc R . . C29 C 0.4458(3) 0.5862(2) 0.3625(3) 0.0632(10) Uani 1 1 d . . . H29 H 0.4578 0.6377 0.3348 0.076 Uiso 1 1 calc R . . C40 C 0.3468(2) 0.0517(3) 0.6113(2) 0.0646(11) Uani 1 1 d . . . H40A H 0.3097 0.1075 0.6245 0.097 Uiso 1 1 calc R . . H40B H 0.3501 0.0137 0.6584 0.097 Uiso 1 1 calc R . . H40C H 0.3212 0.0233 0.5698 0.097 Uiso 1 1 calc R . . C32 C 0.4109(3) 0.4370(2) 0.4415(2) 0.0604(10) Uani 1 1 d . . . H32 H 0.3981 0.3859 0.4695 0.072 Uiso 1 1 calc R . . C26 C 0.3272(3) 0.3775(3) 0.2445(3) 0.0679(11) Uani 1 1 d . . . H26 H 0.3237 0.4325 0.2689 0.082 Uiso 1 1 calc R . . C80 C 1.1533(3) 0.4626(3) 0.4588(3) 0.0790(14) Uani 1 1 d . . . H80A H 1.1066 0.4321 0.4837 0.118 Uiso 1 1 calc R . . H80B H 1.1901 0.4780 0.4993 0.118 Uiso 1 1 calc R . . H80C H 1.1899 0.4243 0.4201 0.118 Uiso 1 1 calc R . . C30 C 0.4046(3) 0.5922(3) 0.4371(3) 0.0673(11) Uani 1 1 d . . . H30 H 0.3874 0.6475 0.4610 0.081 Uiso 1 1 calc R . . C24 C 0.2646(3) 0.2838(3) 0.1614(2) 0.0666(11) Uani 1 1 d . . . H24 H 0.2201 0.2743 0.1282 0.080 Uiso 1 1 calc R . . C19 C 0.3690(3) 0.0398(3) -0.1227(2) 0.0608(10) Uani 1 1 d . . . H19A H 0.3993 0.0514 -0.1739 0.091 Uiso 1 1 calc R . . H19B H 0.3066 0.0374 -0.1295 0.091 Uiso 1 1 calc R . . H19C H 0.3966 -0.0161 -0.1011 0.091 Uiso 1 1 calc R . . C69 C 0.6087(3) 0.7170(3) 0.2127(3) 0.0698(11) Uani 1 1 d . . . H69 H 0.5694 0.7470 0.1771 0.084 Uiso 1 1 calc R . . C11 C 0.7140(3) 0.3649(3) -0.1882(3) 0.0722(12) Uani 1 1 d . . . H11 H 0.6692 0.3931 -0.2197 0.087 Uiso 1 1 calc R . . C79 C 1.1329(3) 0.6231(3) 0.4469(3) 0.0799(14) Uani 1 1 d . . . H79A H 1.1397 0.6632 0.4019 0.120 Uiso 1 1 calc R . . H79B H 1.1879 0.6127 0.4737 0.120 Uiso 1 1 calc R . . H79C H 1.0843 0.6491 0.4838 0.120 Uiso 1 1 calc R . . C71 C 0.6516(3) 0.6909(3) 0.3439(3) 0.0665(11) Uani 1 1 d . . . H71 H 0.6419 0.7026 0.3987 0.080 Uiso 1 1 calc R . . C31 C 0.3885(3) 0.5178(3) 0.4765(3) 0.0770(13) Uani 1 1 d . . . H31 H 0.3614 0.5215 0.5288 0.092 Uiso 1 1 calc R . . C25 C 0.2606(3) 0.3625(3) 0.1971(3) 0.0829(15) Uani 1 1 d . . . H25 H 0.2122 0.4074 0.1896 0.099 Uiso 1 1 calc R . . N2 N 0.43465(19) 0.06744(19) 0.58386(18) 0.0505(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I2 0.03932(10) 0.03516(9) 0.03544(10) 0.00101(7) -0.00572(7) -0.00372(7) I1 0.03443(9) 0.03094(8) 0.03779(10) -0.00201(7) -0.00101(7) -0.00472(7) I4 0.04294(10) 0.03309(9) 0.02958(9) -0.00189(7) -0.00101(7) -0.00269(7) I3 0.03265(9) 0.03608(9) 0.03316(9) -0.00014(7) 0.00310(7) -0.00507(7) Cu2 0.0388(2) 0.0385(2) 0.0405(2) -0.00118(18) 0.00540(18) -0.00314(18) Cu3 0.0381(2) 0.0364(2) 0.0352(2) 0.00130(17) -0.00164(17) -0.00290(18) Cu1 0.0413(2) 0.0422(2) 0.0355(2) -0.00748(18) -0.00208(18) -0.00497(19) Cu4 0.0425(2) 0.0340(2) 0.0379(2) -0.00020(17) -0.00310(18) -0.00909(18) P3 0.0310(3) 0.0314(3) 0.0320(4) 0.0009(3) -0.0014(3) -0.0040(3) P4 0.0373(4) 0.0310(3) 0.0382(4) 0.0015(3) -0.0040(3) -0.0070(3) P1 0.0375(4) 0.0407(4) 0.0338(4) -0.0073(3) -0.0008(3) -0.0030(3) P2 0.0330(4) 0.0352(3) 0.0335(4) -0.0009(3) 0.0013(3) -0.0017(3) C54 0.0350(15) 0.0299(13) 0.0381(16) -0.0010(11) -0.0044(11) -0.0049(11) C56 0.0321(14) 0.0408(15) 0.0309(14) 0.0020(12) -0.0026(11) -0.0079(12) C53 0.0295(14) 0.0348(13) 0.0322(14) 0.0013(11) -0.0037(11) -0.0060(11) C58 0.0350(15) 0.0286(13) 0.0363(15) 0.0046(11) -0.0034(11) -0.0048(11) C13 0.0434(17) 0.0432(16) 0.0326(15) -0.0050(12) -0.0014(12) -0.0068(13) C2 0.0383(16) 0.0428(16) 0.0482(18) -0.0049(14) 0.0032(13) -0.0066(13) C57 0.0355(15) 0.0373(14) 0.0353(15) -0.0003(12) -0.0021(12) -0.0022(12) N3 0.0542(16) 0.0419(14) 0.0380(14) 0.0041(11) 0.0078(12) -0.0049(12) C34 0.0332(15) 0.0430(15) 0.0375(16) -0.0031(13) -0.0013(12) -0.0092(12) C62 0.054(2) 0.0494(18) 0.0422(18) 0.0075(15) -0.0020(14) -0.0149(16) N1 0.0537(18) 0.0596(18) 0.0594(19) -0.0144(15) -0.0068(14) -0.0195(15) C21 0.0393(16) 0.0435(16) 0.0335(15) 0.0016(13) -0.0011(12) -0.0014(13) C47 0.0382(15) 0.0316(13) 0.0331(15) 0.0017(11) 0.0018(11) -0.0021(12) C33 0.0336(15) 0.0383(14) 0.0345(15) -0.0009(12) -0.0001(11) -0.0038(12) C55 0.0391(16) 0.0350(14) 0.0392(16) 0.0052(12) -0.0053(12) -0.0095(12) C61 0.0350(15) 0.0388(15) 0.0430(17) 0.0067(13) -0.0028(12) -0.0061(12) C73 0.0409(16) 0.0337(14) 0.0413(17) 0.0006(12) -0.0030(13) -0.0067(12) C18 0.0490(18) 0.0428(16) 0.0351(16) -0.0028(13) 0.0010(13) -0.0070(14) C7 0.0490(18) 0.0406(15) 0.0358(16) -0.0077(13) -0.0004(13) -0.0041(14) C41 0.0295(14) 0.0294(13) 0.0478(17) 0.0031(12) -0.0028(12) -0.0026(11) C27 0.0334(15) 0.0412(15) 0.0418(17) -0.0051(13) -0.0022(12) -0.0003(12) C36 0.0417(16) 0.0393(15) 0.0394(17) -0.0013(13) -0.0050(13) -0.0093(13) C17 0.059(2) 0.0406(16) 0.0398(17) -0.0061(13) -0.0019(14) -0.0164(15) C37 0.0310(15) 0.0505(17) 0.0409(17) 0.0034(14) -0.0010(12) -0.0110(13) C75 0.058(2) 0.0320(14) 0.0519(19) -0.0021(13) -0.0118(15) -0.0115(14) C78 0.0439(18) 0.0336(14) 0.059(2) -0.0030(14) -0.0112(14) -0.0060(13) C23 0.060(2) 0.0531(19) 0.050(2) -0.0023(16) -0.0118(16) -0.0133(17) C16 0.0499(18) 0.0470(17) 0.0362(16) -0.0015(13) -0.0052(13) -0.0168(15) C45 0.0407(18) 0.0432(17) 0.075(2) -0.0144(17) -0.0149(16) -0.0019(14) C35 0.0341(15) 0.0417(15) 0.0399(16) 0.0020(13) -0.0088(12) -0.0060(12) C38 0.0333(15) 0.0494(17) 0.0389(17) 0.0042(14) -0.0049(12) -0.0024(13) C1 0.0374(16) 0.0410(15) 0.0444(17) -0.0090(13) 0.0015(13) -0.0031(13) C46 0.0377(16) 0.0405(15) 0.0519(19) -0.0055(14) -0.0056(13) -0.0034(13) C77 0.052(2) 0.0358(15) 0.062(2) 0.0003(15) -0.0190(16) -0.0041(14) C67 0.0442(17) 0.0337(14) 0.0504(19) -0.0007(13) -0.0021(14) -0.0088(13) C52 0.0398(16) 0.0423(16) 0.0443(17) -0.0034(13) -0.0050(13) -0.0009(13) C6 0.054(2) 0.0549(19) 0.0442(19) -0.0103(16) 0.0039(15) -0.0034(16) C50 0.060(2) 0.0350(15) 0.0450(19) -0.0035(14) 0.0029(15) 0.0002(15) C22 0.0460(18) 0.0469(17) 0.051(2) -0.0028(15) -0.0090(14) -0.0014(15) N4 0.085(2) 0.0438(16) 0.090(3) -0.0023(16) -0.051(2) -0.0102(16) C76 0.053(2) 0.0425(17) 0.054(2) -0.0032(15) -0.0160(15) -0.0084(15) C60 0.066(2) 0.055(2) 0.0394(18) -0.0002(15) 0.0094(16) -0.0048(17) C8 0.0483(19) 0.061(2) 0.048(2) -0.0020(16) 0.0061(15) -0.0068(16) C68 0.049(2) 0.055(2) 0.055(2) 0.0078(17) -0.0030(16) 0.0022(16) C51 0.0426(18) 0.0410(16) 0.061(2) -0.0036(15) 0.0007(15) 0.0016(14) C44 0.0345(17) 0.0334(15) 0.101(3) -0.0044(18) -0.0105(18) -0.0034(13) C64 0.0434(19) 0.072(2) 0.050(2) 0.0165(18) -0.0055(15) -0.0140(17) C42 0.0381(17) 0.0443(17) 0.059(2) 0.0124(15) -0.0003(14) -0.0028(14) C3 0.0414(18) 0.0445(17) 0.068(2) 0.0017(16) 0.0011(16) -0.0027(15) C66 0.055(2) 0.0493(18) 0.050(2) 0.0052(15) -0.0011(15) -0.0180(16) C65 0.058(2) 0.054(2) 0.067(2) 0.0203(18) -0.0059(18) -0.0227(18) C39 0.057(2) 0.0454(17) 0.050(2) 0.0093(15) -0.0155(16) -0.0070(16) C14 0.0473(19) 0.0514(18) 0.054(2) -0.0211(16) -0.0032(15) -0.0093(15) C15 0.0431(18) 0.0550(19) 0.056(2) -0.0198(16) 0.0000(15) -0.0082(15) C48 0.0450(18) 0.0386(16) 0.059(2) -0.0056(15) -0.0131(15) 0.0014(14) C9 0.064(2) 0.054(2) 0.063(2) -0.0059(18) 0.0190(19) -0.0090(18) C74 0.0500(18) 0.0319(14) 0.0504(19) 0.0019(13) -0.0095(14) -0.0061(13) C59 0.068(2) 0.0503(19) 0.0386(18) 0.0088(15) 0.0060(16) -0.0060(17) C28 0.061(2) 0.0414(17) 0.052(2) -0.0027(15) 0.0026(16) -0.0012(16) C43 0.0357(17) 0.0445(18) 0.086(3) 0.0135(18) 0.0033(17) -0.0061(14) C12 0.061(2) 0.0520(19) 0.057(2) 0.0017(17) -0.0119(17) -0.0113(17) C4 0.0443(19) 0.0454(19) 0.085(3) -0.0137(19) 0.0124(18) 0.0001(15) C10 0.090(3) 0.0440(19) 0.060(2) 0.0043(17) 0.011(2) -0.009(2) C20 0.046(2) 0.078(3) 0.072(3) -0.016(2) -0.0063(18) -0.0231(19) C72 0.059(2) 0.0499(19) 0.052(2) -0.0047(16) -0.0006(16) -0.0045(17) C5 0.056(2) 0.059(2) 0.060(2) -0.0215(19) 0.0138(18) -0.0004(18) C70 0.064(3) 0.049(2) 0.091(3) -0.007(2) 0.013(2) 0.0086(19) C49 0.061(2) 0.0408(17) 0.062(2) -0.0095(16) -0.0178(17) -0.0047(16) C63 0.061(2) 0.070(2) 0.0422(19) 0.0057(17) -0.0042(16) -0.0154(19) C29 0.064(2) 0.0415(18) 0.082(3) -0.0051(19) -0.009(2) -0.0016(17) C40 0.055(2) 0.078(3) 0.066(3) 0.031(2) -0.0130(18) -0.028(2) C32 0.074(3) 0.051(2) 0.051(2) -0.0123(17) 0.0152(18) -0.0033(18) C26 0.078(3) 0.048(2) 0.076(3) -0.0110(19) -0.033(2) 0.0099(19) C80 0.085(3) 0.057(2) 0.102(4) 0.010(2) -0.058(3) -0.011(2) C30 0.063(2) 0.054(2) 0.082(3) -0.030(2) -0.012(2) 0.0097(19) C24 0.063(2) 0.079(3) 0.059(2) -0.004(2) -0.0265(19) -0.005(2) C19 0.068(2) 0.067(2) 0.055(2) -0.0133(18) -0.0080(18) -0.031(2) C69 0.059(2) 0.058(2) 0.084(3) 0.011(2) 0.000(2) 0.0114(19) C11 0.089(3) 0.055(2) 0.073(3) 0.015(2) -0.020(2) -0.008(2) C79 0.091(3) 0.054(2) 0.102(4) -0.015(2) -0.053(3) -0.007(2) C71 0.071(3) 0.060(2) 0.064(3) -0.014(2) 0.009(2) 0.000(2) C31 0.092(3) 0.066(3) 0.066(3) -0.024(2) 0.015(2) 0.003(2) C25 0.083(3) 0.069(3) 0.095(4) -0.010(2) -0.051(3) 0.018(2) N2 0.0461(16) 0.0539(16) 0.0546(17) 0.0190(14) -0.0138(13) -0.0151(13) _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 2.6524(5) . ? I2 Cu4 2.6638(5) . ? I2 Cu1 2.6677(5) . ? I1 Cu2 2.6689(5) . ? I1 Cu3 2.6938(5) . ? I1 Cu1 2.6955(5) . ? I4 Cu4 2.6699(5) . ? I4 Cu3 2.6726(5) . ? I4 Cu2 2.6937(5) . ? I3 Cu1 2.6797(5) . ? I3 Cu4 2.6817(5) . ? I3 Cu3 2.6857(5) . ? Cu2 P2 2.2510(8) . ? Cu2 Cu1 2.8526(6) . ? Cu2 Cu4 2.9394(6) . ? Cu3 P3 2.2524(8) . ? Cu1 P1 2.2533(8) . ? Cu1 Cu4 2.8283(6) . ? Cu4 P4 2.2506(8) . ? P3 C53 1.823(3) . ? P3 C41 1.838(3) . ? P3 C47 1.838(3) . ? P4 C73 1.816(3) . ? P4 C61 1.831(3) . ? P4 C67 1.835(3) . ? P1 C13 1.815(3) . ? P1 C1 1.826(3) . ? P1 C7 1.832(3) . ? P2 C33 1.814(3) . ? P2 C27 1.826(3) . ? P2 C21 1.829(3) . ? C54 C55 1.388(4) . ? C54 C53 1.392(4) . ? C56 N3 1.376(4) . ? C56 C55 1.401(4) . ? C56 C57 1.407(4) . ? C53 C58 1.389(4) . ? C58 C57 1.384(4) . ? C13 C14 1.386(5) . ? C13 C18 1.389(4) . ? C2 C3 1.388(5) . ? C2 C1 1.392(5) . ? N3 C60 1.445(4) . ? N3 C59 1.446(4) . ? C34 C35 1.380(4) . ? C34 C33 1.394(4) . ? C62 C61 1.381(5) . ? C62 C63 1.387(5) . ? N1 C16 1.370(4) . ? N1 C20 1.434(5) . ? N1 C19 1.452(4) . ? C21 C26 1.381(5) . ? C21 C22 1.389(5) . ? C47 C52 1.383(4) . ? C47 C48 1.389(4) . ? C33 C38 1.393(4) . ? C61 C66 1.392(4) . ? C73 C78 1.393(4) . ? C73 C74 1.399(4) . ? C18 C17 1.379(5) . ? C7 C12 1.387(5) . ? C7 C8 1.391(5) . ? C41 C46 1.390(4) . ? C41 C42 1.393(4) . ? C27 C28 1.380(5) . ? C27 C32 1.381(5) . ? C36 N2 1.367(4) . ? C36 C37 1.411(4) . ? C36 C35 1.413(4) . ? C17 C16 1.402(5) . ? C37 C38 1.372(4) . ? C75 C74 1.381(4) . ? C75 C76 1.408(5) . ? C78 C77 1.381(4) . ? C23 C24 1.367(5) . ? C23 C22 1.386(5) . ? C16 C15 1.408(4) . ? C45 C44 1.372(5) . ? C45 C46 1.389(4) . ? C1 C6 1.391(5) . ? C77 C76 1.408(4) . ? C67 C68 1.390(5) . ? C67 C72 1.391(5) . ? C52 C51 1.396(4) . ? C6 C5 1.389(5) . ? C50 C51 1.366(5) . ? C50 C49 1.386(5) . ? N4 C76 1.364(4) . ? N4 C79 1.439(5) . ? N4 C80 1.453(5) . ? C8 C9 1.378(5) . ? C68 C69 1.391(5) . ? C44 C43 1.372(6) . ? C64 C65 1.375(6) . ? C64 C63 1.376(5) . ? C42 C43 1.392(5) . ? C3 C4 1.389(5) . ? C66 C65 1.386(5) . ? C39 N2 1.451(4) . ? C14 C15 1.382(5) . ? C48 C49 1.382(5) . ? C9 C10 1.379(6) . ? C28 C29 1.390(5) . ? C12 C11 1.385(5) . ? C4 C5 1.386(6) . ? C10 C11 1.371(6) . ? C72 C71 1.387(5) . ? C70 C71 1.365(6) . ? C70 C69 1.382(6) . ? C29 C30 1.370(6) . ? C40 N2 1.445(4) . ? C32 C31 1.384(5) . ? C26 C25 1.401(6) . ? C30 C31 1.362(6) . ? C24 C25 1.366(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu2 I2 Cu4 67.136(14) . . ? Cu2 I2 Cu1 64.849(14) . . ? Cu4 I2 Cu1 64.076(14) . . ? Cu2 I1 Cu3 70.101(14) . . ? Cu2 I1 Cu1 64.248(14) . . ? Cu3 I1 Cu1 69.269(14) . . ? Cu4 I4 Cu3 70.116(13) . . ? Cu4 I4 Cu2 66.463(14) . . ? Cu3 I4 Cu2 70.048(14) . . ? Cu1 I3 Cu4 63.677(14) . . ? Cu1 I3 Cu3 69.621(14) . . ? Cu4 I3 Cu3 69.743(13) . . ? P2 Cu2 I2 115.43(3) . . ? P2 Cu2 I1 104.22(2) . . ? I2 Cu2 I1 112.177(17) . . ? P2 Cu2 I4 110.01(3) . . ? I2 Cu2 I4 108.121(16) . . ? I1 Cu2 I4 106.514(16) . . ? P2 Cu2 Cu1 145.65(3) . . ? I2 Cu2 Cu1 57.836(13) . . ? I1 Cu2 Cu1 58.328(13) . . ? I4 Cu2 Cu1 103.626(17) . . ? P2 Cu2 Cu4 150.88(3) . . ? I2 Cu2 Cu4 56.618(12) . . ? I1 Cu2 Cu4 104.469(16) . . ? I4 Cu2 Cu4 56.379(13) . . ? Cu1 Cu2 Cu4 58.435(15) . . ? P3 Cu3 I4 111.39(2) . . ? P3 Cu3 I3 113.42(2) . . ? I4 Cu3 I3 106.227(15) . . ? P3 Cu3 I1 113.04(2) . . ? I4 Cu3 I1 106.405(15) . . ? I3 Cu3 I1 105.828(16) . . ? P1 Cu1 I2 110.06(3) . . ? P1 Cu1 I3 108.42(3) . . ? I2 Cu1 I3 112.474(16) . . ? P1 Cu1 I1 108.94(3) . . ? I2 Cu1 I1 110.854(16) . . ? I3 Cu1 I1 105.951(16) . . ? P1 Cu1 Cu4 144.12(3) . . ? I2 Cu1 Cu4 57.894(13) . . ? I3 Cu1 Cu4 58.195(13) . . ? I1 Cu1 Cu4 106.847(17) . . ? P1 Cu1 Cu2 144.18(3) . . ? I2 Cu1 Cu2 57.315(13) . . ? I3 Cu1 Cu2 107.281(17) . . ? I1 Cu1 Cu2 57.424(13) . . ? Cu4 Cu1 Cu2 62.318(15) . . ? P4 Cu4 I2 109.14(3) . . ? P4 Cu4 I4 102.91(2) . . ? I2 Cu4 I4 108.493(16) . . ? P4 Cu4 I3 116.60(3) . . ? I2 Cu4 I3 112.538(16) . . ? I4 Cu4 I3 106.422(15) . . ? P4 Cu4 Cu1 151.94(3) . . ? I2 Cu4 Cu1 58.030(13) . . ? I4 Cu4 Cu1 104.914(17) . . ? I3 Cu4 Cu1 58.128(13) . . ? P4 Cu4 Cu2 138.14(3) . . ? I2 Cu4 Cu2 56.246(13) . . ? I4 Cu4 Cu2 57.158(13) . . ? I3 Cu4 Cu2 104.803(16) . . ? Cu1 Cu4 Cu2 59.247(15) . . ? C53 P3 C41 102.88(13) . . ? C53 P3 C47 104.04(13) . . ? C41 P3 C47 103.55(13) . . ? C53 P3 Cu3 114.23(9) . . ? C41 P3 Cu3 114.53(9) . . ? C47 P3 Cu3 116.05(10) . . ? C73 P4 C61 106.32(14) . . ? C73 P4 C67 103.25(14) . . ? C61 P4 C67 103.53(14) . . ? C73 P4 Cu4 116.13(10) . . ? C61 P4 Cu4 114.55(10) . . ? C67 P4 Cu4 111.73(10) . . ? C13 P1 C1 104.05(14) . . ? C13 P1 C7 104.68(15) . . ? C1 P1 C7 103.03(15) . . ? C13 P1 Cu1 113.47(10) . . ? C1 P1 Cu1 117.08(11) . . ? C7 P1 Cu1 113.17(10) . . ? C33 P2 C27 104.48(14) . . ? C33 P2 C21 101.40(14) . . ? C27 P2 C21 104.39(14) . . ? C33 P2 Cu2 117.13(10) . . ? C27 P2 Cu2 112.71(10) . . ? C21 P2 Cu2 115.18(10) . . ? C55 C54 C53 120.9(3) . . ? N3 C56 C55 122.0(3) . . ? N3 C56 C57 120.9(3) . . ? C55 C56 C57 117.1(3) . . ? C58 C53 C54 118.2(3) . . ? C58 C53 P3 117.9(2) . . ? C54 C53 P3 123.9(2) . . ? C57 C58 C53 121.3(3) . . ? C14 C13 C18 116.7(3) . . ? C14 C13 P1 118.6(2) . . ? C18 C13 P1 124.7(2) . . ? C3 C2 C1 120.7(3) . . ? C58 C57 C56 121.1(3) . . ? C56 N3 C60 119.7(3) . . ? C56 N3 C59 120.5(3) . . ? C60 N3 C59 119.1(3) . . ? C35 C34 C33 121.8(3) . . ? C61 C62 C63 121.4(3) . . ? C16 N1 C20 122.9(3) . . ? C16 N1 C19 119.1(3) . . ? C20 N1 C19 118.0(3) . . ? C26 C21 C22 117.8(3) . . ? C26 C21 P2 124.2(3) . . ? C22 C21 P2 118.0(2) . . ? C52 C47 C48 119.0(3) . . ? C52 C47 P3 122.9(2) . . ? C48 C47 P3 118.1(2) . . ? C34 C33 C38 117.0(3) . . ? C34 C33 P2 120.3(2) . . ? C38 C33 P2 122.6(2) . . ? C54 C55 C56 121.4(3) . . ? C62 C61 C66 118.4(3) . . ? C62 C61 P4 118.2(2) . . ? C66 C61 P4 123.3(3) . . ? C78 C73 C74 116.7(3) . . ? C78 C73 P4 119.2(2) . . ? C74 C73 P4 124.0(2) . . ? C17 C18 C13 121.7(3) . . ? C12 C7 C8 118.6(3) . . ? C12 C7 P1 122.2(3) . . ? C8 C7 P1 119.0(3) . . ? C46 C41 C42 118.5(3) . . ? C46 C41 P3 122.5(2) . . ? C42 C41 P3 119.0(3) . . ? C28 C27 C32 118.8(3) . . ? C28 C27 P2 119.0(2) . . ? C32 C27 P2 122.1(3) . . ? N2 C36 C37 121.0(3) . . ? N2 C36 C35 122.3(3) . . ? C37 C36 C35 116.7(3) . . ? C18 C17 C16 121.6(3) . . ? C38 C37 C36 121.1(3) . . ? C74 C75 C76 121.4(3) . . ? C77 C78 C73 122.3(3) . . ? C24 C23 C22 120.5(3) . . ? N1 C16 C17 122.3(3) . . ? N1 C16 C15 121.1(3) . . ? C17 C16 C15 116.6(3) . . ? C44 C45 C46 120.1(4) . . ? C34 C35 C36 121.1(3) . . ? C37 C38 C33 122.3(3) . . ? C6 C1 C2 118.6(3) . . ? C6 C1 P1 123.1(3) . . ? C2 C1 P1 118.2(2) . . ? C41 C46 C45 120.8(3) . . ? C78 C77 C76 121.0(3) . . ? C68 C67 C72 118.8(3) . . ? C68 C67 P4 120.4(3) . . ? C72 C67 P4 120.6(3) . . ? C47 C52 C51 120.1(3) . . ? C5 C6 C1 120.8(4) . . ? C51 C50 C49 119.6(3) . . ? C23 C22 C21 121.0(3) . . ? C76 N4 C79 121.5(3) . . ? C76 N4 C80 120.5(3) . . ? C79 N4 C80 116.8(3) . . ? N4 C76 C75 121.5(3) . . ? N4 C76 C77 121.7(3) . . ? C75 C76 C77 116.8(3) . . ? C9 C8 C7 120.9(4) . . ? C67 C68 C69 120.2(4) . . ? C50 C51 C52 120.5(3) . . ? C45 C44 C43 119.8(3) . . ? C65 C64 C63 120.2(3) . . ? C43 C42 C41 120.0(3) . . ? C2 C3 C4 120.2(4) . . ? C65 C66 C61 120.2(3) . . ? C64 C65 C66 120.3(3) . . ? C15 C14 C13 122.6(3) . . ? C14 C15 C16 120.5(3) . . ? C49 C48 C47 120.5(3) . . ? C8 C9 C10 120.1(4) . . ? C75 C74 C73 121.8(3) . . ? C27 C28 C29 120.1(4) . . ? C44 C43 C42 120.7(3) . . ? C7 C12 C11 119.9(4) . . ? C5 C4 C3 119.5(3) . . ? C11 C10 C9 119.3(4) . . ? C71 C72 C67 120.3(4) . . ? C4 C5 C6 120.2(3) . . ? C71 C70 C69 120.0(4) . . ? C48 C49 C50 120.3(3) . . ? C62 C63 C64 119.4(4) . . ? C30 C29 C28 120.6(4) . . ? C31 C32 C27 120.2(4) . . ? C21 C26 C25 120.7(4) . . ? C31 C30 C29 119.2(4) . . ? C25 C24 C23 119.4(4) . . ? C70 C69 C68 120.0(4) . . ? C10 C11 C12 121.1(4) . . ? C70 C71 C72 120.5(4) . . ? C30 C31 C32 121.0(4) . . ? C24 C25 C26 120.5(4) . . ? C36 N2 C40 120.8(3) . . ? C36 N2 C39 121.7(3) . . ? C40 N2 C39 117.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.60 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.563 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.063 _database_code_depnum_ccdc_archive 'CCDC 915489' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form ###END data_1\170K #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 4(C20H20N1P1Cu1I1) _chemical_formula_sum 'C80 H80 Cu4 I4 N4 P4' _chemical_formula_weight 1983.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3594(4) _cell_length_b 15.4883(4) _cell_length_c 16.9959(5) _cell_angle_alpha 88.447(2) _cell_angle_beta 85.484(2) _cell_angle_gamma 81.238(2) _cell_volume 3983.11(19) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 23500 _cell_measurement_theta_min 2.6060 _cell_measurement_theta_max 74.0649 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2653 _exptl_crystal_size_mid 0.2031 _exptl_crystal_size_min 0.1483 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 14.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68844 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5992 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42805 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 66.59 _reflns_number_total 14062 _reflns_number_gt 12415 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _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^)+(0.0361P)^2^+2.4386P] 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 14062 _refine_ls_number_parameters 873 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 I3 I 0.899683(15) 0.258803(15) 0.149453(13) 0.03639(6) Uani 1 1 d . . . I4 I 0.737537(16) 0.362408(15) 0.351986(13) 0.03758(6) Uani 1 1 d . . . I1 I 0.670592(15) 0.144571(14) 0.230576(14) 0.03653(6) Uani 1 1 d . . . I2 I 0.632832(16) 0.408952(15) 0.123132(14) 0.03888(6) Uani 1 1 d . . . Cu2 Cu 0.62246(4) 0.31525(4) 0.25553(3) 0.04206(13) Uani 1 1 d . . . Cu3 Cu 0.80710(4) 0.21326(4) 0.28067(3) 0.03906(12) Uani 1 1 d . . . Cu4 Cu 0.77938(4) 0.39402(4) 0.19959(3) 0.04051(13) Uani 1 1 d . . . Cu1 Cu 0.73224(4) 0.25195(4) 0.11921(3) 0.04215(13) Uani 1 1 d . . . P3 P 0.88869(6) 0.12248(6) 0.36169(5) 0.03349(19) Uani 1 1 d . . . P2 P 0.48701(6) 0.32507(6) 0.31870(6) 0.0366(2) Uani 1 1 d . . . P4 P 0.82564(6) 0.52501(6) 0.20112(6) 0.0372(2) Uani 1 1 d . . . P1 P 0.73267(7) 0.19214(7) -0.00015(6) 0.0393(2) Uani 1 1 d . . . C68 C 0.8635(3) 0.5135(3) 0.0399(3) 0.0509(10) Uani 1 1 d . . . H68 H 0.8441 0.4582 0.0470 0.061 Uiso 1 1 calc R . . C2 C 0.8412(3) 0.0404(3) 0.0417(3) 0.0455(9) Uani 1 1 d . . . H2 H 0.8223 0.0577 0.0942 0.055 Uiso 1 1 calc R . . C58 C 0.7885(3) 0.1739(2) 0.4989(2) 0.0374(8) Uani 1 1 d . . . H58 H 0.7873 0.2306 0.4760 0.045 Uiso 1 1 calc R . . C28 C 0.4707(3) 0.5051(3) 0.3276(3) 0.0560(11) Uani 1 1 d . . . H28 H 0.5010 0.5013 0.2766 0.067 Uiso 1 1 calc R . . C74 C 0.9627(3) 0.4577(3) 0.2926(3) 0.0443(9) Uani 1 1 d . . . H74 H 0.9513 0.4028 0.2756 0.053 Uiso 1 1 calc R . . C14 C 0.5504(3) 0.2126(3) 0.0097(3) 0.0552(11) Uani 1 1 d . . . H14 H 0.5551 0.2609 0.0415 0.066 Uiso 1 1 calc R . . C61 C 0.7359(3) 0.6111(2) 0.2365(2) 0.0426(9) Uani 1 1 d . . . C56 C 0.7482(2) 0.0813(2) 0.6096(2) 0.0361(8) Uani 1 1 d . . . C32 C 0.4106(4) 0.4369(3) 0.4417(3) 0.0650(13) Uani 1 1 d . . . H32 H 0.3977 0.3859 0.4698 0.078 Uiso 1 1 calc R . . C46 C 1.0063(3) 0.1699(3) 0.4680(3) 0.0448(9) Uani 1 1 d . . . H46 H 0.9674 0.1514 0.5091 0.054 Uiso 1 1 calc R . . C54 C 0.8310(2) 0.0202(2) 0.4914(2) 0.0367(8) Uani 1 1 d . . . H54 H 0.8599 -0.0298 0.4636 0.044 Uiso 1 1 calc R . . C18 C 0.6171(3) 0.0882(3) -0.0621(2) 0.0463(9) Uani 1 1 d . . . H18 H 0.6682 0.0495 -0.0808 0.056 Uiso 1 1 calc R . . C13 C 0.6276(3) 0.1604(3) -0.0199(2) 0.0398(8) Uani 1 1 d . . . C17 C 0.5357(3) 0.0706(3) -0.0780(2) 0.0477(10) Uani 1 1 d . . . H17 H 0.5317 0.0204 -0.1076 0.057 Uiso 1 1 calc R . . C67 C 0.8622(2) 0.5661(3) 0.1040(3) 0.0420(9) Uani 1 1 d . . . C72 C 0.8906(3) 0.6467(3) 0.0919(3) 0.0541(11) Uani 1 1 d . . . H72 H 0.8899 0.6843 0.1352 0.065 Uiso 1 1 calc R . . C42 C 1.0463(3) 0.1894(3) 0.3301(3) 0.0491(10) Uani 1 1 d . . . H42 H 1.0348 0.1851 0.2763 0.059 Uiso 1 1 calc R . . C1 C 0.8122(3) 0.0938(3) -0.0218(2) 0.0423(9) Uani 1 1 d . . . C48 C 0.8751(3) -0.0277(3) 0.2811(3) 0.0477(10) Uani 1 1 d . . . H48 H 0.8176 0.0013 0.2719 0.057 Uiso 1 1 calc R . . C27 C 0.4518(3) 0.4301(3) 0.3661(2) 0.0402(8) Uani 1 1 d . . . C7 C 0.7564(3) 0.2662(3) -0.0824(2) 0.0431(9) Uani 1 1 d . . . N2 N 0.4344(2) 0.0675(3) 0.5842(2) 0.0530(9) Uani 1 1 d . . . C76 C 1.0479(3) 0.5388(3) 0.3699(3) 0.0504(10) Uani 1 1 d . . . C50 C 0.9873(3) -0.1535(3) 0.2636(3) 0.0508(10) Uani 1 1 d . . . H50 H 1.0070 -0.2098 0.2423 0.061 Uiso 1 1 calc R . . C33 C 0.4715(3) 0.2448(2) 0.3966(2) 0.0386(8) Uani 1 1 d . . . C51 C 1.0413(3) -0.1141(3) 0.3068(3) 0.0533(11) Uani 1 1 d . . . H51 H 1.0984 -0.1440 0.3163 0.064 Uiso 1 1 calc R . . C45 C 1.0805(3) 0.2043(3) 0.4866(3) 0.0557(11) Uani 1 1 d . . . H45 H 1.0920 0.2098 0.5403 0.067 Uiso 1 1 calc R . . C36 C 0.4467(3) 0.1256(3) 0.5235(2) 0.0403(8) Uani 1 1 d . . . C34 C 0.5413(2) 0.2077(3) 0.4386(2) 0.0382(8) Uani 1 1 d . . . H34 H 0.5984 0.2222 0.4246 0.046 Uiso 1 1 calc R . . C38 C 0.3880(3) 0.2207(3) 0.4177(2) 0.0433(9) Uani 1 1 d . . . H38 H 0.3390 0.2446 0.3890 0.052 Uiso 1 1 calc R . . C39 C 0.5068(3) 0.0274(3) 0.6285(3) 0.0555(11) Uani 1 1 d . . . H39A H 0.5582 0.0076 0.5921 0.083 Uiso 1 1 calc R . . H39B H 0.4894 -0.0227 0.6590 0.083 Uiso 1 1 calc R . . H39C H 0.5220 0.0701 0.6646 0.083 Uiso 1 1 calc R . . C5 C 0.8991(3) -0.0095(3) -0.1106(3) 0.0608(12) Uani 1 1 d . . . H5 H 0.9193 -0.0264 -0.1630 0.073 Uiso 1 1 calc R . . C52 C 1.0139(3) -0.0310(3) 0.3370(3) 0.0464(9) Uani 1 1 d . . . H52 H 1.0523 -0.0042 0.3665 0.056 Uiso 1 1 calc R . . C37 C 0.3762(3) 0.1629(3) 0.4793(3) 0.0456(9) Uani 1 1 d . . . H37 H 0.3191 0.1479 0.4923 0.055 Uiso 1 1 calc R . . C69 C 0.8928(3) 0.5398(3) -0.0355(3) 0.0578(11) Uani 1 1 d . . . H69 H 0.8940 0.5025 -0.0792 0.069 Uiso 1 1 calc R . . C35 C 0.5302(3) 0.1497(3) 0.5008(2) 0.0435(9) Uani 1 1 d . . . H35 H 0.5797 0.1257 0.5287 0.052 Uiso 1 1 calc R . . C20 C 0.3692(4) 0.0399(3) -0.1225(3) 0.0643(13) Uani 1 1 d . . . H20A H 0.4013 0.0504 -0.1732 0.096 Uiso 1 1 calc R . . H20B H 0.3070 0.0386 -0.1307 0.096 Uiso 1 1 calc R . . H20C H 0.3951 -0.0162 -0.1000 0.096 Uiso 1 1 calc R . . C57 C 0.7478(2) 0.1648(2) 0.5739(2) 0.0378(8) Uani 1 1 d . . . H57 H 0.7193 0.2151 0.6015 0.045 Uiso 1 1 calc R . . C55 C 0.7901(3) 0.0093(2) 0.5658(2) 0.0399(8) Uani 1 1 d . . . H55 H 0.7903 -0.0480 0.5875 0.048 Uiso 1 1 calc R . . C41 C 0.9887(3) 0.1624(2) 0.3898(3) 0.0420(9) Uani 1 1 d . . . C49 C 0.9037(3) -0.1105(3) 0.2515(3) 0.0594(12) Uani 1 1 d . . . H49 H 0.8655 -0.1380 0.2225 0.071 Uiso 1 1 calc R . . C66 C 0.7208(3) 0.6286(3) 0.3160(3) 0.0567(11) Uani 1 1 d . . . H66 H 0.7585 0.5972 0.3522 0.068 Uiso 1 1 calc R . . C3 C 0.8974(3) -0.0374(3) 0.0281(3) 0.0560(11) Uani 1 1 d . . . H3 H 0.9163 -0.0735 0.0715 0.067 Uiso 1 1 calc R . . C53 C 0.8311(2) 0.1023(2) 0.4565(2) 0.0337(7) Uani 1 1 d . . . C22 C 0.4005(3) 0.2335(3) 0.2201(3) 0.0530(11) Uani 1 1 d . . . H22 H 0.4488 0.1884 0.2267 0.064 Uiso 1 1 calc R . . C60 C 0.6734(3) 0.1486(3) 0.7293(3) 0.0567(12) Uani 1 1 d . . . H60A H 0.7215 0.1815 0.7377 0.085 Uiso 1 1 calc R . . H60B H 0.6470 0.1308 0.7804 0.085 Uiso 1 1 calc R . . H60C H 0.6282 0.1855 0.7007 0.085 Uiso 1 1 calc R . . C75 C 1.0279(3) 0.4594(3) 0.3433(3) 0.0552(11) Uani 1 1 d . . . H75 H 1.0600 0.4059 0.3606 0.066 Uiso 1 1 calc R . . N3 N 0.7077(3) 0.0723(2) 0.6838(2) 0.0500(9) Uani 1 1 d . . . N1 N 0.3756(3) 0.1093(3) -0.0687(2) 0.0560(9) Uani 1 1 d . . . C16 C 0.4579(3) 0.1249(3) -0.0515(2) 0.0455(9) Uani 1 1 d . . . C21 C 0.3978(3) 0.3132(3) 0.2565(2) 0.0421(9) Uani 1 1 d . . . C73 C 0.9132(3) 0.5334(2) 0.2655(2) 0.0406(8) Uani 1 1 d . . . C59 C 0.7118(4) -0.0127(3) 0.7218(3) 0.0595(12) Uani 1 1 d . . . H59A H 0.6877 -0.0523 0.6882 0.089 Uiso 1 1 calc R . . H59B H 0.6771 -0.0073 0.7728 0.089 Uiso 1 1 calc R . . H59C H 0.7734 -0.0361 0.7301 0.089 Uiso 1 1 calc R . . C47 C 0.9301(2) 0.0129(2) 0.3241(2) 0.0355(8) Uani 1 1 d . . . C78 C 0.9317(3) 0.6125(3) 0.2920(3) 0.0459(9) Uani 1 1 d . . . H78 H 0.8985 0.6655 0.2748 0.055 Uiso 1 1 calc R . . C71 C 0.9199(3) 0.6726(3) 0.0173(3) 0.0605(12) Uani 1 1 d . . . H71 H 0.9402 0.7275 0.0100 0.073 Uiso 1 1 calc R . . C23 C 0.3335(3) 0.2190(3) 0.1741(3) 0.0554(11) Uani 1 1 d . . . H23 H 0.3353 0.1634 0.1512 0.066 Uiso 1 1 calc R . . N4 N 1.1135(3) 0.5416(3) 0.4194(3) 0.0730(13) Uani 1 1 d . . . C77 C 0.9972(3) 0.6155(3) 0.3427(3) 0.0503(10) Uani 1 1 d . . . H77 H 1.0083 0.6706 0.3594 0.060 Uiso 1 1 calc R . . C6 C 0.8433(3) 0.0679(3) -0.0978(3) 0.0560(11) Uani 1 1 d . . . H6 H 0.8259 0.1043 -0.1415 0.067 Uiso 1 1 calc R . . C44 C 1.1374(3) 0.2305(3) 0.4270(4) 0.0608(13) Uani 1 1 d . . . H44 H 1.1882 0.2540 0.4396 0.073 Uiso 1 1 calc R . . C62 C 0.6779(3) 0.6541(3) 0.1848(3) 0.0579(12) Uani 1 1 d . . . H62 H 0.6853 0.6404 0.1303 0.069 Uiso 1 1 calc R . . C19 C 0.2958(3) 0.1614(4) -0.0383(3) 0.0662(14) Uani 1 1 d . . . H19A H 0.2911 0.1569 0.0194 0.099 Uiso 1 1 calc R . . H19B H 0.2451 0.1405 -0.0590 0.099 Uiso 1 1 calc R . . H19C H 0.2965 0.2225 -0.0545 0.099 Uiso 1 1 calc R . . C43 C 1.1212(3) 0.2227(3) 0.3496(3) 0.0594(13) Uani 1 1 d . . . H43 H 1.1611 0.2402 0.3089 0.071 Uiso 1 1 calc R . . C70 C 0.9199(3) 0.6201(3) -0.0460(3) 0.0584(12) Uani 1 1 d . . . H70 H 0.9388 0.6391 -0.0973 0.070 Uiso 1 1 calc R . . C15 C 0.4676(3) 0.1964(3) -0.0058(3) 0.0545(11) Uani 1 1 d . . . H15 H 0.4167 0.2341 0.0146 0.065 Uiso 1 1 calc R . . C12 C 0.8421(3) 0.2869(3) -0.0941(3) 0.0564(11) Uani 1 1 d . . . H12 H 0.8864 0.2612 -0.0611 0.068 Uiso 1 1 calc R . . C8 C 0.6937(4) 0.3060(3) -0.1289(3) 0.0596(12) Uani 1 1 d . . . H8 H 0.6351 0.2933 -0.1210 0.072 Uiso 1 1 calc R . . C11 C 0.8624(4) 0.3447(3) -0.1537(3) 0.0638(13) Uani 1 1 d . . . H11 H 0.9209 0.3579 -0.1618 0.077 Uiso 1 1 calc R . . C4 C 0.9260(3) -0.0628(3) -0.0477(3) 0.0635(14) Uani 1 1 d . . . H4 H 0.9639 -0.1166 -0.0567 0.076 Uiso 1 1 calc R . . C26 C 0.3274(4) 0.3772(3) 0.2446(3) 0.0711(15) Uani 1 1 d . . . H26 H 0.3236 0.4322 0.2691 0.085 Uiso 1 1 calc R . . C10 C 0.7989(4) 0.3830(3) -0.2015(3) 0.0718(15) Uani 1 1 d . . . H10 H 0.8134 0.4216 -0.2432 0.086 Uiso 1 1 calc R . . C29 C 0.4459(4) 0.5865(3) 0.3625(4) 0.0675(14) Uani 1 1 d . . . H29 H 0.4574 0.6381 0.3347 0.081 Uiso 1 1 calc R . . C24 C 0.2656(4) 0.2832(4) 0.1617(3) 0.0670(14) Uani 1 1 d . . . H24 H 0.2210 0.2737 0.1287 0.080 Uiso 1 1 calc R . . C64 C 0.5971(4) 0.7359(3) 0.2919(4) 0.0703(15) Uani 1 1 d . . . H64 H 0.5507 0.7800 0.3105 0.084 Uiso 1 1 calc R . . C63 C 0.6091(3) 0.7169(4) 0.2125(3) 0.0692(14) Uani 1 1 d . . . H63 H 0.5702 0.7471 0.1767 0.083 Uiso 1 1 calc R . . C30 C 0.4049(4) 0.5918(4) 0.4372(4) 0.0724(16) Uani 1 1 d . . . H30 H 0.3880 0.6470 0.4615 0.087 Uiso 1 1 calc R . . C80 C 1.1529(4) 0.4626(4) 0.4592(4) 0.0802(18) Uani 1 1 d . . . H80A H 1.1062 0.4345 0.4873 0.120 Uiso 1 1 calc R . . H80B H 1.1929 0.4776 0.4971 0.120 Uiso 1 1 calc R . . H80C H 1.1860 0.4224 0.4202 0.120 Uiso 1 1 calc R . . C40 C 0.3469(3) 0.0517(4) 0.6109(3) 0.0725(16) Uani 1 1 d . . . H40A H 0.3101 0.1071 0.6255 0.109 Uiso 1 1 calc R . . H40B H 0.3501 0.0121 0.6569 0.109 Uiso 1 1 calc R . . H40C H 0.3210 0.0250 0.5685 0.109 Uiso 1 1 calc R . . C9 C 0.7141(4) 0.3651(4) -0.1881(4) 0.0744(15) Uani 1 1 d . . . H9 H 0.6692 0.3931 -0.2195 0.089 Uiso 1 1 calc R . . C65 C 0.6519(4) 0.6910(4) 0.3440(4) 0.0707(14) Uani 1 1 d . . . H65 H 0.6426 0.7027 0.3989 0.085 Uiso 1 1 calc R . . C79 C 1.1317(4) 0.6231(4) 0.4473(4) 0.086(2) Uani 1 1 d . . . H79A H 1.1400 0.6627 0.4023 0.129 Uiso 1 1 calc R . . H79B H 1.1855 0.6129 0.4757 0.129 Uiso 1 1 calc R . . H79C H 1.0820 0.6495 0.4828 0.129 Uiso 1 1 calc R . . C31 C 0.3884(4) 0.5175(4) 0.4763(4) 0.0825(18) Uani 1 1 d . . . H31 H 0.3610 0.5213 0.5285 0.099 Uiso 1 1 calc R . . C25 C 0.2618(4) 0.3624(4) 0.1971(4) 0.090(2) Uani 1 1 d . . . H25 H 0.2138 0.4074 0.1891 0.108 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 I3 0.03496(12) 0.03817(12) 0.03500(12) 0.00001(9) 0.00373(9) -0.00557(9) I4 0.04567(13) 0.03467(11) 0.03118(12) -0.00157(9) -0.00077(9) -0.00306(10) I1 0.03706(12) 0.03256(11) 0.03969(13) -0.00182(9) -0.00089(9) -0.00518(9) I2 0.04182(13) 0.03718(12) 0.03743(13) 0.00142(9) -0.00594(9) -0.00416(10) Cu2 0.0406(3) 0.0407(3) 0.0427(3) -0.0007(2) 0.0054(2) -0.0035(2) Cu3 0.0401(3) 0.0390(3) 0.0369(3) 0.0019(2) -0.0019(2) -0.0029(2) Cu4 0.0465(3) 0.0362(3) 0.0400(3) -0.0001(2) -0.0022(2) -0.0103(2) Cu1 0.0442(3) 0.0447(3) 0.0373(3) -0.0073(2) -0.0020(2) -0.0053(3) P3 0.0325(4) 0.0334(4) 0.0340(5) 0.0011(4) -0.0012(3) -0.0041(4) P2 0.0356(5) 0.0370(5) 0.0351(5) -0.0007(4) 0.0018(4) -0.0014(4) P4 0.0394(5) 0.0329(4) 0.0402(5) 0.0023(4) -0.0051(4) -0.0072(4) P1 0.0385(5) 0.0424(5) 0.0363(5) -0.0080(4) -0.0013(4) -0.0032(4) C68 0.059(3) 0.049(2) 0.047(2) 0.0079(19) -0.007(2) -0.016(2) C2 0.039(2) 0.045(2) 0.052(2) -0.0058(19) 0.0066(17) -0.0084(18) C58 0.043(2) 0.0313(17) 0.038(2) 0.0028(15) -0.0017(16) -0.0055(15) C28 0.069(3) 0.041(2) 0.054(3) -0.002(2) 0.005(2) -0.001(2) C74 0.043(2) 0.0355(19) 0.056(3) -0.0001(18) -0.0166(18) -0.0042(17) C14 0.046(2) 0.057(3) 0.064(3) -0.025(2) -0.003(2) -0.008(2) C61 0.045(2) 0.0342(19) 0.049(2) 0.0005(17) -0.0013(17) -0.0078(17) C56 0.0313(18) 0.0399(19) 0.038(2) 0.0028(16) -0.0055(15) -0.0073(15) C32 0.082(4) 0.054(3) 0.056(3) -0.014(2) 0.015(3) -0.006(3) C46 0.038(2) 0.045(2) 0.052(2) -0.0021(18) -0.0108(18) -0.0018(17) C54 0.0369(19) 0.0331(18) 0.041(2) -0.0016(15) -0.0046(15) -0.0064(15) C18 0.056(3) 0.042(2) 0.040(2) -0.0055(17) 0.0059(18) -0.0090(19) C13 0.041(2) 0.047(2) 0.0320(19) -0.0017(16) -0.0089(15) -0.0055(17) C17 0.058(3) 0.043(2) 0.044(2) -0.0082(18) -0.0026(19) -0.016(2) C67 0.0269(18) 0.042(2) 0.057(2) 0.0071(18) -0.0040(16) -0.0045(16) C72 0.062(3) 0.051(2) 0.051(3) 0.005(2) 0.001(2) -0.019(2) C42 0.038(2) 0.050(2) 0.057(3) 0.015(2) -0.0047(18) -0.0015(18) C1 0.038(2) 0.045(2) 0.044(2) -0.0078(17) 0.0019(16) -0.0061(17) C48 0.045(2) 0.038(2) 0.060(3) -0.0027(19) -0.0161(19) 0.0005(17) C27 0.036(2) 0.041(2) 0.043(2) -0.0046(17) -0.0016(16) -0.0013(16) C7 0.046(2) 0.044(2) 0.038(2) -0.0096(17) 0.0025(17) -0.0023(18) N2 0.046(2) 0.060(2) 0.057(2) 0.0208(18) -0.0153(17) -0.0171(17) C76 0.055(3) 0.044(2) 0.055(3) -0.0007(19) -0.019(2) -0.0091(19) C50 0.063(3) 0.036(2) 0.051(3) -0.0047(18) 0.001(2) -0.0025(19) C33 0.040(2) 0.0392(19) 0.036(2) -0.0011(16) 0.0018(15) -0.0060(16) C51 0.047(2) 0.045(2) 0.064(3) -0.003(2) 0.001(2) 0.0045(19) C45 0.049(3) 0.047(2) 0.072(3) -0.012(2) -0.018(2) -0.003(2) C36 0.040(2) 0.041(2) 0.041(2) 0.0051(17) -0.0113(16) -0.0091(17) C34 0.0282(18) 0.044(2) 0.043(2) -0.0039(17) 0.0002(15) -0.0078(16) C38 0.0321(19) 0.052(2) 0.045(2) 0.0042(18) -0.0039(16) -0.0065(17) C39 0.068(3) 0.047(2) 0.052(3) 0.009(2) -0.014(2) -0.009(2) C5 0.059(3) 0.065(3) 0.054(3) -0.018(2) 0.015(2) 0.001(2) C52 0.042(2) 0.044(2) 0.052(2) -0.0033(18) -0.0065(18) -0.0009(18) C37 0.035(2) 0.054(2) 0.049(2) 0.0045(19) -0.0008(17) -0.0156(18) C69 0.057(3) 0.073(3) 0.044(2) 0.006(2) -0.005(2) -0.014(2) C35 0.038(2) 0.045(2) 0.048(2) -0.0004(18) -0.0047(17) -0.0077(17) C20 0.072(3) 0.070(3) 0.059(3) -0.014(2) -0.005(2) -0.033(3) C57 0.0371(19) 0.0374(19) 0.037(2) -0.0018(15) 0.0018(15) -0.0006(16) C55 0.044(2) 0.0366(19) 0.040(2) 0.0062(16) -0.0060(16) -0.0094(16) C41 0.036(2) 0.0308(18) 0.058(3) 0.0017(17) -0.0011(17) -0.0041(15) C49 0.070(3) 0.042(2) 0.068(3) -0.012(2) -0.019(2) -0.003(2) C66 0.062(3) 0.052(3) 0.055(3) -0.002(2) -0.002(2) -0.002(2) C3 0.046(2) 0.046(2) 0.073(3) 0.001(2) 0.007(2) -0.004(2) C53 0.0301(18) 0.0386(18) 0.0331(19) 0.0001(15) -0.0023(14) -0.0073(15) C22 0.059(3) 0.048(2) 0.052(3) -0.001(2) -0.012(2) -0.006(2) C60 0.065(3) 0.058(3) 0.043(2) -0.002(2) 0.016(2) -0.004(2) C75 0.059(3) 0.035(2) 0.072(3) -0.003(2) -0.016(2) -0.0044(19) N3 0.059(2) 0.0459(19) 0.0418(19) 0.0037(15) 0.0133(16) -0.0075(17) N1 0.049(2) 0.061(2) 0.063(2) -0.0143(19) -0.0094(17) -0.0189(18) C16 0.056(2) 0.048(2) 0.036(2) -0.0005(17) -0.0059(18) -0.018(2) C21 0.044(2) 0.047(2) 0.035(2) 0.0018(17) 0.0012(16) -0.0056(18) C73 0.044(2) 0.0344(18) 0.044(2) 0.0000(16) -0.0058(17) -0.0071(16) C59 0.074(3) 0.053(3) 0.049(3) 0.009(2) 0.008(2) -0.009(2) C47 0.0381(19) 0.0344(18) 0.0319(19) 0.0020(15) 0.0023(15) -0.0023(15) C78 0.049(2) 0.037(2) 0.053(2) 0.0041(18) -0.0160(19) -0.0054(18) C71 0.059(3) 0.056(3) 0.070(3) 0.018(2) -0.005(2) -0.023(2) C23 0.064(3) 0.057(3) 0.049(3) 0.000(2) -0.019(2) -0.011(2) N4 0.083(3) 0.047(2) 0.097(3) -0.001(2) -0.051(3) -0.011(2) C77 0.063(3) 0.034(2) 0.057(3) 0.0002(18) -0.012(2) -0.0120(19) C6 0.060(3) 0.057(3) 0.048(3) -0.014(2) 0.008(2) -0.004(2) C44 0.039(2) 0.034(2) 0.111(4) -0.002(2) -0.015(3) -0.0023(18) C62 0.044(2) 0.059(3) 0.067(3) 0.004(2) -0.001(2) 0.001(2) C19 0.050(3) 0.081(4) 0.073(3) -0.016(3) -0.006(2) -0.024(3) C43 0.038(2) 0.047(2) 0.092(4) 0.014(2) -0.001(2) -0.0077(19) C70 0.046(2) 0.078(3) 0.052(3) 0.022(2) -0.006(2) -0.016(2) C15 0.046(2) 0.059(3) 0.060(3) -0.020(2) -0.002(2) -0.012(2) C12 0.053(3) 0.066(3) 0.047(3) 0.004(2) 0.005(2) -0.006(2) C8 0.066(3) 0.054(3) 0.060(3) 0.004(2) -0.010(2) -0.011(2) C11 0.062(3) 0.059(3) 0.067(3) -0.003(2) 0.016(2) -0.006(2) C4 0.045(3) 0.049(3) 0.093(4) -0.018(3) 0.013(2) -0.003(2) C26 0.074(3) 0.056(3) 0.082(4) -0.009(3) -0.039(3) 0.012(3) C10 0.101(4) 0.046(3) 0.064(3) 0.005(2) 0.012(3) -0.010(3) C29 0.071(3) 0.043(2) 0.087(4) -0.007(2) -0.010(3) -0.001(2) C24 0.063(3) 0.081(4) 0.060(3) -0.004(3) -0.029(2) -0.008(3) C64 0.059(3) 0.054(3) 0.090(4) -0.004(3) 0.006(3) 0.008(2) C63 0.057(3) 0.067(3) 0.077(4) 0.020(3) -0.013(3) 0.011(3) C30 0.066(3) 0.058(3) 0.091(4) -0.033(3) -0.015(3) 0.011(3) C80 0.078(4) 0.061(3) 0.109(5) 0.006(3) -0.052(4) -0.011(3) C40 0.063(3) 0.087(4) 0.072(4) 0.039(3) -0.014(3) -0.029(3) C9 0.093(4) 0.056(3) 0.074(4) 0.015(3) -0.020(3) -0.009(3) C65 0.076(4) 0.062(3) 0.070(4) -0.017(3) 0.010(3) -0.003(3) C79 0.101(5) 0.057(3) 0.106(5) -0.016(3) -0.064(4) -0.002(3) C31 0.093(4) 0.073(4) 0.075(4) -0.029(3) 0.014(3) 0.004(3) C25 0.094(5) 0.073(4) 0.101(5) -0.012(3) -0.060(4) 0.021(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 I3 Cu1 2.6804(6) . ? I3 Cu4 2.6826(6) . ? I3 Cu3 2.6859(6) . ? I4 Cu4 2.6695(6) . ? I4 Cu3 2.6726(6) . ? I4 Cu2 2.6943(7) . ? I1 Cu2 2.6703(6) . ? I1 Cu3 2.6949(6) . ? I1 Cu1 2.6966(6) . ? I2 Cu2 2.6518(6) . ? I2 Cu4 2.6635(6) . ? I2 Cu1 2.6666(6) . ? Cu2 P2 2.2505(11) . ? Cu2 Cu1 2.8595(8) . ? Cu2 Cu4 2.9450(8) . ? Cu3 P3 2.2525(11) . ? Cu4 P4 2.2509(11) . ? Cu4 Cu1 2.8350(8) . ? Cu1 P1 2.2520(11) . ? P3 C53 1.820(4) . ? P3 C47 1.833(4) . ? P3 C41 1.841(4) . ? P2 C33 1.819(4) . ? P2 C27 1.822(4) . ? P2 C21 1.829(4) . ? P4 C73 1.822(4) . ? P4 C67 1.831(4) . ? P4 C61 1.842(4) . ? P1 C13 1.815(4) . ? P1 C1 1.828(4) . ? P1 C7 1.833(4) . ? C68 C67 1.375(6) . ? C68 C69 1.395(6) . ? C2 C3 1.384(6) . ? C2 C1 1.399(6) . ? C58 C53 1.387(5) . ? C58 C57 1.389(5) . ? C28 C27 1.376(6) . ? C28 C29 1.396(7) . ? C74 C75 1.375(6) . ? C74 C73 1.386(5) . ? C14 C15 1.380(6) . ? C14 C13 1.396(6) . ? C61 C66 1.381(6) . ? C61 C62 1.385(6) . ? C56 N3 1.374(5) . ? C56 C55 1.402(5) . ? C56 C57 1.412(5) . ? C32 C31 1.378(7) . ? C32 C27 1.387(6) . ? C46 C41 1.389(6) . ? C46 C45 1.391(6) . ? C54 C55 1.385(5) . ? C54 C53 1.389(5) . ? C18 C17 1.369(6) . ? C18 C13 1.381(6) . ? C17 C16 1.403(6) . ? C67 C72 1.389(6) . ? C72 C71 1.380(7) . ? C42 C41 1.393(6) . ? C42 C43 1.396(6) . ? C1 C6 1.390(6) . ? C48 C49 1.385(6) . ? C48 C47 1.389(6) . ? C7 C8 1.359(6) . ? C7 C12 1.400(6) . ? N2 C36 1.372(5) . ? N2 C40 1.438(6) . ? N2 C39 1.445(5) . ? C76 N4 1.368(6) . ? C76 C75 1.407(6) . ? C76 C77 1.407(6) . ? C50 C51 1.369(7) . ? C50 C49 1.381(7) . ? C33 C34 1.378(5) . ? C33 C38 1.406(5) . ? C51 C52 1.391(6) . ? C45 C44 1.379(7) . ? C36 C37 1.407(6) . ? C36 C35 1.412(6) . ? C34 C35 1.385(6) . ? C38 C37 1.378(6) . ? C5 C6 1.375(7) . ? C5 C4 1.385(8) . ? C52 C47 1.392(5) . ? C69 C70 1.374(7) . ? C20 N1 1.449(6) . ? C66 C65 1.384(7) . ? C3 C4 1.376(7) . ? C22 C21 1.389(6) . ? C22 C23 1.387(6) . ? C60 N3 1.438(6) . ? N3 C59 1.446(6) . ? N1 C16 1.377(6) . ? N1 C19 1.429(6) . ? C16 C15 1.402(6) . ? C21 C26 1.375(6) . ? C73 C78 1.392(5) . ? C78 C77 1.382(6) . ? C71 C70 1.367(7) . ? C23 C24 1.353(7) . ? N4 C79 1.435(6) . ? N4 C80 1.455(6) . ? C44 C43 1.369(8) . ? C62 C63 1.385(7) . ? C12 C11 1.382(7) . ? C8 C9 1.391(7) . ? C11 C10 1.373(8) . ? C26 C25 1.388(7) . ? C10 C9 1.373(8) . ? C29 C30 1.371(8) . ? C24 C25 1.371(8) . ? C64 C65 1.372(8) . ? C64 C63 1.381(8) . ? C30 C31 1.360(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 I3 Cu4 63.825(18) . . ? Cu1 I3 Cu3 69.726(18) . . ? Cu4 I3 Cu3 69.816(18) . . ? Cu4 I4 Cu3 70.211(18) . . ? Cu4 I4 Cu2 66.603(18) . . ? Cu3 I4 Cu2 70.139(18) . . ? Cu2 I1 Cu3 70.165(18) . . ? Cu2 I1 Cu1 64.387(18) . . ? Cu3 I1 Cu1 69.352(18) . . ? Cu2 I2 Cu4 67.291(18) . . ? Cu2 I2 Cu1 65.048(18) . . ? Cu4 I2 Cu1 64.265(18) . . ? P2 Cu2 I2 115.48(3) . . ? P2 Cu2 I1 104.33(3) . . ? I2 Cu2 I1 112.04(2) . . ? P2 Cu2 I4 110.14(3) . . ? I2 Cu2 I4 108.03(2) . . ? I1 Cu2 I4 106.46(2) . . ? P2 Cu2 Cu1 145.61(4) . . ? I2 Cu2 Cu1 57.726(17) . . ? I1 Cu2 Cu1 58.253(17) . . ? I4 Cu2 Cu1 103.55(2) . . ? P2 Cu2 Cu4 150.86(4) . . ? I2 Cu2 Cu4 56.544(16) . . ? I1 Cu2 Cu4 104.40(2) . . ? I4 Cu2 Cu4 56.296(17) . . ? Cu1 Cu2 Cu4 58.450(19) . . ? P3 Cu3 I4 111.48(3) . . ? P3 Cu3 I3 113.43(3) . . ? I4 Cu3 I3 106.18(2) . . ? P3 Cu3 I1 113.05(3) . . ? I4 Cu3 I1 106.38(2) . . ? I3 Cu3 I1 105.78(2) . . ? P4 Cu4 I2 109.31(3) . . ? P4 Cu4 I4 102.97(3) . . ? I2 Cu4 I4 108.42(2) . . ? P4 Cu4 I3 116.63(3) . . ? I2 Cu4 I3 112.40(2) . . ? I4 Cu4 I3 106.37(2) . . ? P4 Cu4 Cu1 151.93(4) . . ? I2 Cu4 Cu1 57.920(17) . . ? I4 Cu4 Cu1 104.86(2) . . ? I3 Cu4 Cu1 58.049(17) . . ? P4 Cu4 Cu2 138.18(4) . . ? I2 Cu4 Cu2 56.165(17) . . ? I4 Cu4 Cu2 57.102(17) . . ? I3 Cu4 Cu2 104.73(2) . . ? Cu1 Cu4 Cu2 59.266(19) . . ? P1 Cu1 I2 110.18(3) . . ? P1 Cu1 I3 108.51(3) . . ? I2 Cu1 I3 112.37(2) . . ? P1 Cu1 I1 109.01(3) . . ? I2 Cu1 I1 110.74(2) . . ? I3 Cu1 I1 105.89(2) . . ? P1 Cu1 Cu4 144.15(4) . . ? I2 Cu1 Cu4 57.815(17) . . ? I3 Cu1 Cu4 58.126(17) . . ? I1 Cu1 Cu4 106.75(2) . . ? P1 Cu1 Cu2 144.19(4) . . ? I2 Cu1 Cu2 57.226(17) . . ? I3 Cu1 Cu2 107.17(2) . . ? I1 Cu1 Cu2 57.360(17) . . ? Cu4 Cu1 Cu2 62.28(2) . . ? C53 P3 C47 104.01(17) . . ? C53 P3 C41 102.97(18) . . ? C47 P3 C41 103.74(17) . . ? C53 P3 Cu3 114.07(12) . . ? C47 P3 Cu3 116.00(13) . . ? C41 P3 Cu3 114.52(13) . . ? C33 P2 C27 104.38(18) . . ? C33 P2 C21 101.64(18) . . ? C27 P2 C21 104.34(18) . . ? C33 P2 Cu2 116.86(13) . . ? C27 P2 Cu2 112.71(13) . . ? C21 P2 Cu2 115.37(13) . . ? C73 P4 C67 106.37(18) . . ? C73 P4 C61 103.63(19) . . ? C67 P4 C61 103.41(18) . . ? C73 P4 Cu4 116.09(13) . . ? C67 P4 Cu4 114.48(14) . . ? C61 P4 Cu4 111.57(13) . . ? C13 P1 C1 103.68(18) . . ? C13 P1 C7 104.18(19) . . ? C1 P1 C7 103.08(18) . . ? C13 P1 Cu1 113.75(13) . . ? C1 P1 Cu1 117.29(14) . . ? C7 P1 Cu1 113.37(13) . . ? C67 C68 C69 121.2(4) . . ? C3 C2 C1 120.3(4) . . ? C53 C58 C57 121.8(3) . . ? C27 C28 C29 120.8(5) . . ? C75 C74 C73 122.0(4) . . ? C15 C14 C13 122.2(4) . . ? C66 C61 C62 118.9(4) . . ? C66 C61 P4 120.3(3) . . ? C62 C61 P4 120.6(3) . . ? N3 C56 C55 122.2(3) . . ? N3 C56 C57 120.6(3) . . ? C55 C56 C57 117.2(3) . . ? C31 C32 C27 120.2(5) . . ? C41 C46 C45 120.5(4) . . ? C55 C54 C53 121.7(4) . . ? C17 C18 C13 122.2(4) . . ? C18 C13 C14 116.6(4) . . ? C18 C13 P1 125.4(3) . . ? C14 C13 P1 118.0(3) . . ? C18 C17 C16 121.6(4) . . ? C68 C67 C72 118.3(4) . . ? C68 C67 P4 118.2(3) . . ? C72 C67 P4 123.5(3) . . ? C71 C72 C67 120.6(5) . . ? C41 C42 C43 119.6(5) . . ? C6 C1 C2 118.4(4) . . ? C6 C1 P1 123.5(4) . . ? C2 C1 P1 118.1(3) . . ? C49 C48 C47 120.2(4) . . ? C28 C27 C32 118.4(4) . . ? C28 C27 P2 119.2(3) . . ? C32 C27 P2 122.3(3) . . ? C8 C7 C12 118.6(4) . . ? C8 C7 P1 123.2(4) . . ? C12 C7 P1 118.1(3) . . ? C36 N2 C40 120.5(4) . . ? C36 N2 C39 121.5(4) . . ? C40 N2 C39 117.7(4) . . ? N4 C76 C75 122.0(4) . . ? N4 C76 C77 121.5(4) . . ? C75 C76 C77 116.5(4) . . ? C51 C50 C49 119.2(4) . . ? C34 C33 C38 117.9(4) . . ? C34 C33 P2 120.6(3) . . ? C38 C33 P2 121.5(3) . . ? C50 C51 C52 121.0(4) . . ? C44 C45 C46 119.8(5) . . ? N2 C36 C37 121.2(4) . . ? N2 C36 C35 122.2(4) . . ? C37 C36 C35 116.6(4) . . ? C33 C34 C35 121.7(3) . . ? C37 C38 C33 120.9(4) . . ? C6 C5 C4 120.4(4) . . ? C47 C52 C51 119.9(4) . . ? C38 C37 C36 121.7(4) . . ? C70 C69 C68 119.4(5) . . ? C34 C35 C36 121.2(4) . . ? C58 C57 C56 120.6(3) . . ? C54 C55 C56 121.1(3) . . ? C46 C41 C42 119.3(4) . . ? C46 C41 P3 122.4(3) . . ? C42 C41 P3 118.2(3) . . ? C50 C49 C48 120.8(4) . . ? C61 C66 C65 121.1(5) . . ? C4 C3 C2 120.5(5) . . ? C58 C53 C54 117.6(3) . . ? C58 C53 P3 118.0(3) . . ? C54 C53 P3 124.3(3) . . ? C21 C22 C23 120.9(4) . . ? C74 C75 C76 121.4(4) . . ? C56 N3 C60 119.9(3) . . ? C56 N3 C59 120.5(4) . . ? C60 N3 C59 118.8(4) . . ? C16 N1 C19 122.6(4) . . ? C16 N1 C20 119.1(4) . . ? C19 N1 C20 118.3(4) . . ? N1 C16 C17 122.2(4) . . ? N1 C16 C15 121.1(4) . . ? C17 C16 C15 116.7(4) . . ? C26 C21 C22 117.8(4) . . ? C26 C21 P2 124.4(3) . . ? C22 C21 P2 117.8(3) . . ? C74 C73 C78 117.4(4) . . ? C74 C73 P4 119.1(3) . . ? C78 C73 P4 123.5(3) . . ? C48 C47 C52 119.0(4) . . ? C48 C47 P3 118.3(3) . . ? C52 C47 P3 122.7(3) . . ? C77 C78 C73 121.4(4) . . ? C70 C71 C72 120.5(4) . . ? C24 C23 C22 120.5(5) . . ? C76 N4 C79 121.2(4) . . ? C76 N4 C80 120.4(4) . . ? C79 N4 C80 117.0(4) . . ? C78 C77 C76 121.4(4) . . ? C5 C6 C1 120.9(5) . . ? C43 C44 C45 120.3(4) . . ? C63 C62 C61 120.0(5) . . ? C44 C43 C42 120.6(5) . . ? C71 C70 C69 120.0(4) . . ? C14 C15 C16 120.7(4) . . ? C11 C12 C7 120.2(5) . . ? C7 C8 C9 121.1(5) . . ? C10 C11 C12 120.6(5) . . ? C3 C4 C5 119.5(4) . . ? C21 C26 C25 120.7(5) . . ? C9 C10 C11 119.3(5) . . ? C30 C29 C28 119.7(5) . . ? C23 C24 C25 119.4(5) . . ? C65 C64 C63 120.1(5) . . ? C64 C63 C62 120.2(5) . . ? C31 C30 C29 119.6(5) . . ? C10 C9 C8 120.3(5) . . ? C64 C65 C66 119.5(5) . . ? C30 C31 C32 121.2(6) . . ? C24 C25 C26 120.6(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.59 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.630 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.076 _database_code_depnum_ccdc_archive 'CCDC 915490' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form ###END data_1\200K #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 4(C20H20N1P1Cu1I1) _chemical_formula_sum 'C80 H80 Cu4 I4 N4 P4' _chemical_formula_weight 1983.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3915(3) _cell_length_b 15.5053(4) _cell_length_c 17.0242(4) _cell_angle_alpha 88.460(2) _cell_angle_beta 85.486(2) _cell_angle_gamma 81.260(2) _cell_volume 4002.73(16) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 22606 _cell_measurement_theta_min 2.6017 _cell_measurement_theta_max 74.0709 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2653 _exptl_crystal_size_mid 0.2031 _exptl_crystal_size_min 0.1483 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 14.397 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0523 _exptl_absorpt_correction_T_max 0.0985 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5992 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43074 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 66.60 _reflns_number_total 14131 _reflns_number_gt 12275 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _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^)+(0.0320P)^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 14131 _refine_ls_number_parameters 873 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.004 _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 0.633123(13) 0.408328(12) 0.123652(11) 0.04253(5) Uani 1 1 d . . . I1 I 0.670946(12) 0.144571(12) 0.230729(11) 0.03966(5) Uani 1 1 d . . . I4 I 0.737694(13) 0.362274(12) 0.351830(11) 0.04086(5) Uani 1 1 d . . . I3 I 0.899287(12) 0.258927(12) 0.149522(11) 0.03970(5) Uani 1 1 d . . . Cu2 Cu 0.62243(3) 0.31497(3) 0.25616(3) 0.04665(11) Uani 1 1 d . . . Cu3 Cu 0.80725(3) 0.21304(3) 0.28076(3) 0.04291(10) Uani 1 1 d . . . Cu1 Cu 0.73242(3) 0.25149(3) 0.11901(3) 0.04647(11) Uani 1 1 d . . . Cu4 Cu 0.77957(3) 0.39437(3) 0.19960(3) 0.04451(11) Uani 1 1 d . . . P4 P 0.82566(5) 0.52527(5) 0.20106(5) 0.04073(17) Uani 1 1 d . . . P3 P 0.88870(5) 0.12241(5) 0.36161(4) 0.03653(15) Uani 1 1 d . . . P2 P 0.48714(5) 0.32508(5) 0.31908(5) 0.03984(16) Uani 1 1 d . . . P1 P 0.73297(5) 0.19209(5) -0.00034(5) 0.04283(17) Uani 1 1 d . . . C58 C 0.8315(2) 0.01985(19) 0.49136(18) 0.0393(6) Uani 1 1 d . . . H58 H 0.8609 -0.0301 0.4639 0.047 Uiso 1 1 calc R . . C56 C 0.7479(2) 0.0815(2) 0.60891(18) 0.0399(6) Uani 1 1 d . . . C55 C 0.7479(2) 0.1643(2) 0.57331(18) 0.0418(7) Uani 1 1 d . . . H55 H 0.7198 0.2147 0.6009 0.050 Uiso 1 1 calc R . . C54 C 0.7883(2) 0.17350(19) 0.49876(18) 0.0400(6) Uani 1 1 d . . . H54 H 0.7865 0.2302 0.4759 0.048 Uiso 1 1 calc R . . C53 C 0.83137(19) 0.10215(19) 0.45636(17) 0.0372(6) Uani 1 1 d . . . C8 C 0.8405(2) 0.0406(2) 0.0405(2) 0.0503(8) Uani 1 1 d . . . H8 H 0.8208 0.0575 0.0929 0.060 Uiso 1 1 calc R . . C57 C 0.7901(2) 0.0093(2) 0.56503(19) 0.0432(7) Uani 1 1 d . . . H57 H 0.7900 -0.0478 0.5866 0.052 Uiso 1 1 calc R . . C13 C 0.6282(2) 0.1603(2) -0.01997(18) 0.0446(7) Uani 1 1 d . . . C18 C 0.6181(2) 0.0882(2) -0.06277(18) 0.0477(7) Uani 1 1 d . . . H18 H 0.6691 0.0500 -0.0820 0.057 Uiso 1 1 calc R . . C38 C 0.5408(2) 0.2076(2) 0.43906(19) 0.0420(7) Uani 1 1 d . . . H38 H 0.5979 0.2220 0.4249 0.050 Uiso 1 1 calc R . . N2 N 0.4341(2) 0.0677(2) 0.58396(19) 0.0584(8) Uani 1 1 d . . . C73 C 0.9125(2) 0.5339(2) 0.2651(2) 0.0446(7) Uani 1 1 d . . . C33 C 0.4706(2) 0.2450(2) 0.39657(18) 0.0407(7) Uani 1 1 d . . . C21 C 0.3989(2) 0.3129(2) 0.25636(19) 0.0452(7) Uani 1 1 d . . . C47 C 0.9883(2) 0.16246(19) 0.3896(2) 0.0431(7) Uani 1 1 d . . . C1 C 0.7571(2) 0.2664(2) -0.0820(2) 0.0493(8) Uani 1 1 d . . . N1 N 0.3773(2) 0.1084(2) -0.0688(2) 0.0627(8) Uani 1 1 d . . . N3 N 0.7080(2) 0.07193(19) 0.68290(17) 0.0542(7) Uani 1 1 d . . . C77 C 0.9967(2) 0.6158(2) 0.3424(2) 0.0540(8) Uani 1 1 d . . . H77 H 1.0080 0.6708 0.3590 0.065 Uiso 1 1 calc R . . C41 C 0.9303(2) 0.01299(19) 0.32400(18) 0.0397(6) Uani 1 1 d . . . C67 C 0.8623(2) 0.5664(2) 0.1042(2) 0.0460(7) Uani 1 1 d . . . C16 C 0.4585(2) 0.1247(2) -0.05166(19) 0.0481(8) Uani 1 1 d . . . C36 C 0.4464(2) 0.1258(2) 0.52368(19) 0.0446(7) Uani 1 1 d . . . C17 C 0.5366(2) 0.0705(2) -0.0781(2) 0.0517(8) Uani 1 1 d . . . H17 H 0.5327 0.0201 -0.1074 0.062 Uiso 1 1 calc R . . C34 C 0.3886(2) 0.2209(2) 0.41817(19) 0.0479(8) Uani 1 1 d . . . H34 H 0.3398 0.2448 0.3896 0.057 Uiso 1 1 calc R . . C27 C 0.4516(2) 0.4303(2) 0.36610(19) 0.0446(7) Uani 1 1 d . . . C52 C 1.0065(2) 0.1703(2) 0.4673(2) 0.0507(8) Uani 1 1 d . . . H52 H 0.9681 0.1517 0.5087 0.061 Uiso 1 1 calc R . . C7 C 0.8124(2) 0.0939(2) -0.0217(2) 0.0468(7) Uani 1 1 d . . . C37 C 0.5297(2) 0.1501(2) 0.50130(19) 0.0452(7) Uani 1 1 d . . . H37 H 0.5790 0.1265 0.5294 0.054 Uiso 1 1 calc R . . C35 C 0.3758(2) 0.1635(2) 0.4797(2) 0.0485(8) Uani 1 1 d . . . H35 H 0.3186 0.1490 0.4927 0.058 Uiso 1 1 calc R . . C12 C 0.8433(3) 0.0686(3) -0.0979(2) 0.0594(9) Uani 1 1 d . . . H12 H 0.8256 0.1048 -0.1416 0.071 Uiso 1 1 calc R . . C76 C 1.0471(2) 0.5389(2) 0.3700(2) 0.0543(8) Uani 1 1 d . . . C61 C 0.7363(2) 0.6109(2) 0.2368(2) 0.0493(8) Uani 1 1 d . . . C68 C 0.8628(3) 0.5147(2) 0.0399(2) 0.0565(9) Uani 1 1 d . . . H68 H 0.8426 0.4599 0.0468 0.068 Uiso 1 1 calc R . . C10 C 0.9258(3) -0.0626(3) -0.0479(3) 0.0674(11) Uani 1 1 d . . . H10 H 0.9634 -0.1165 -0.0570 0.081 Uiso 1 1 calc R . . C23 C 0.3345(3) 0.2193(3) 0.1744(2) 0.0629(10) Uani 1 1 d . . . H23 H 0.3366 0.1639 0.1512 0.076 Uiso 1 1 calc R . . C28 C 0.4107(3) 0.4370(3) 0.4414(2) 0.0690(11) Uani 1 1 d . . . H28 H 0.3981 0.3859 0.4694 0.083 Uiso 1 1 calc R . . C22 C 0.4003(3) 0.2334(2) 0.2205(2) 0.0568(9) Uani 1 1 d . . . H22 H 0.4478 0.1878 0.2279 0.068 Uiso 1 1 calc R . . C46 C 1.0132(2) -0.0311(2) 0.3374(2) 0.0517(8) Uani 1 1 d . . . H46 H 1.0511 -0.0045 0.3674 0.062 Uiso 1 1 calc R . . C59 C 0.6726(3) 0.1482(3) 0.7285(2) 0.0637(10) Uani 1 1 d . . . H59A H 0.7202 0.1813 0.7376 0.096 Uiso 1 1 calc R . . H59B H 0.6457 0.1301 0.7791 0.096 Uiso 1 1 calc R . . H59C H 0.6279 0.1850 0.6995 0.096 Uiso 1 1 calc R . . C45 C 1.0412(2) -0.1137(2) 0.3073(2) 0.0580(9) Uani 1 1 d . . . H45 H 1.0983 -0.1431 0.3168 0.070 Uiso 1 1 calc R . . N4 N 1.1125(3) 0.5416(2) 0.4194(2) 0.0798(11) Uani 1 1 d . . . C42 C 0.8758(2) -0.0274(2) 0.2805(2) 0.0556(9) Uani 1 1 d . . . H42 H 0.8187 0.0020 0.2708 0.067 Uiso 1 1 calc R . . C44 C 0.9875(3) -0.1535(2) 0.2638(2) 0.0557(9) Uani 1 1 d . . . H44 H 1.0072 -0.2098 0.2427 0.067 Uiso 1 1 calc R . . C51 C 1.0802(2) 0.2050(2) 0.4854(3) 0.0623(10) Uani 1 1 d . . . H51 H 1.0913 0.2111 0.5389 0.075 Uiso 1 1 calc R . . C15 C 0.4683(2) 0.1962(3) -0.0056(2) 0.0596(9) Uani 1 1 d . . . H15 H 0.4176 0.2337 0.0153 0.071 Uiso 1 1 calc R . . C72 C 0.8910(3) 0.6468(2) 0.0924(2) 0.0604(9) Uani 1 1 d . . . H72 H 0.8909 0.6839 0.1359 0.072 Uiso 1 1 calc R . . C14 C 0.5514(2) 0.2120(2) 0.0095(2) 0.0575(9) Uani 1 1 d . . . H14 H 0.5562 0.2602 0.0413 0.069 Uiso 1 1 calc R . . C40 C 0.5060(3) 0.0276(2) 0.6287(2) 0.0598(9) Uani 1 1 d . . . H40A H 0.5579 0.0088 0.5928 0.090 Uiso 1 1 calc R . . H40B H 0.4887 -0.0231 0.6581 0.090 Uiso 1 1 calc R . . H40C H 0.5200 0.0699 0.6657 0.090 Uiso 1 1 calc R . . C2 C 0.8418(3) 0.2877(3) -0.0941(2) 0.0626(10) Uani 1 1 d . . . H2 H 0.8860 0.2624 -0.0610 0.075 Uiso 1 1 calc R . . C66 C 0.6786(3) 0.6541(3) 0.1850(3) 0.0644(10) Uani 1 1 d . . . H66 H 0.6866 0.6411 0.1305 0.077 Uiso 1 1 calc R . . C48 C 1.0463(2) 0.1893(2) 0.3298(2) 0.0556(9) Uani 1 1 d . . . H48 H 1.0350 0.1850 0.2761 0.067 Uiso 1 1 calc R . . C70 C 0.9203(3) 0.6207(3) -0.0455(2) 0.0670(11) Uani 1 1 d . . . H70 H 0.9401 0.6394 -0.0965 0.080 Uiso 1 1 calc R . . C75 C 1.0277(2) 0.4595(2) 0.3428(2) 0.0573(9) Uani 1 1 d . . . H75 H 1.0601 0.4061 0.3597 0.069 Uiso 1 1 calc R . . C71 C 0.9198(3) 0.6734(3) 0.0178(3) 0.0688(11) Uani 1 1 d . . . H71 H 0.9394 0.7285 0.0105 0.083 Uiso 1 1 calc R . . C50 C 1.1370(2) 0.2304(2) 0.4267(3) 0.0676(12) Uani 1 1 d . . . H50 H 1.1877 0.2536 0.4394 0.081 Uiso 1 1 calc R . . C32 C 0.4710(3) 0.5049(2) 0.3273(2) 0.0617(10) Uani 1 1 d . . . H32 H 0.5011 0.5012 0.2763 0.074 Uiso 1 1 calc R . . C78 C 0.9319(2) 0.6130(2) 0.2921(2) 0.0511(8) Uani 1 1 d . . . H78 H 0.8991 0.6662 0.2751 0.061 Uiso 1 1 calc R . . C11 C 0.8997(3) -0.0091(3) -0.1103(3) 0.0676(11) Uani 1 1 d . . . H11 H 0.9207 -0.0258 -0.1625 0.081 Uiso 1 1 calc R . . C9 C 0.8970(2) -0.0373(2) 0.0278(3) 0.0620(10) Uani 1 1 d . . . H9 H 0.9157 -0.0730 0.0713 0.074 Uiso 1 1 calc R . . C69 C 0.8922(3) 0.5408(3) -0.0355(2) 0.0692(11) Uani 1 1 d . . . H69 H 0.8928 0.5039 -0.0792 0.083 Uiso 1 1 calc R . . C60 C 0.7119(3) -0.0126(3) 0.7209(2) 0.0626(10) Uani 1 1 d . . . H60A H 0.6887 -0.0525 0.6871 0.094 Uiso 1 1 calc R . . H60B H 0.6765 -0.0072 0.7714 0.094 Uiso 1 1 calc R . . H60C H 0.7733 -0.0355 0.7300 0.094 Uiso 1 1 calc R . . C49 C 1.1207(2) 0.2223(3) 0.3493(3) 0.0687(12) Uani 1 1 d . . . H49 H 1.1608 0.2395 0.3087 0.082 Uiso 1 1 calc R . . C26 C 0.3284(3) 0.3772(3) 0.2443(3) 0.0798(14) Uani 1 1 d . . . H26 H 0.3242 0.4318 0.2693 0.096 Uiso 1 1 calc R . . C4 C 0.7987(4) 0.3830(3) -0.2010(3) 0.0785(13) Uani 1 1 d . . . H4 H 0.8130 0.4216 -0.2426 0.094 Uiso 1 1 calc R . . C6 C 0.6935(3) 0.3060(3) -0.1295(2) 0.0643(10) Uani 1 1 d . . . H6 H 0.6351 0.2930 -0.1220 0.077 Uiso 1 1 calc R . . C24 C 0.2663(3) 0.2840(3) 0.1616(3) 0.0773(13) Uani 1 1 d . . . H24 H 0.2215 0.2742 0.1291 0.093 Uiso 1 1 calc R . . C62 C 0.7209(3) 0.6279(3) 0.3166(2) 0.0640(10) Uani 1 1 d . . . H62 H 0.7580 0.5963 0.3529 0.077 Uiso 1 1 calc R . . C3 C 0.8624(3) 0.3452(3) -0.1534(3) 0.0719(12) Uani 1 1 d . . . H3 H 0.9207 0.3586 -0.1614 0.086 Uiso 1 1 calc R . . C43 C 0.9042(3) -0.1102(2) 0.2514(2) 0.0642(10) Uani 1 1 d . . . H43 H 0.8659 -0.1376 0.2225 0.077 Uiso 1 1 calc R . . C31 C 0.4463(3) 0.5859(3) 0.3626(3) 0.0756(12) Uani 1 1 d . . . H31 H 0.4586 0.6374 0.3351 0.091 Uiso 1 1 calc R . . C19 C 0.3702(3) 0.0395(3) -0.1225(2) 0.0697(11) Uani 1 1 d . . . H19A H 0.4002 0.0511 -0.1738 0.105 Uiso 1 1 calc R . . H19B H 0.3079 0.0372 -0.1288 0.105 Uiso 1 1 calc R . . H19C H 0.3979 -0.0165 -0.1012 0.105 Uiso 1 1 calc R . . C39 C 0.3461(3) 0.0518(3) 0.6106(3) 0.0794(14) Uani 1 1 d . . . H39A H 0.3092 0.1072 0.6248 0.119 Uiso 1 1 calc R . . H39B H 0.3490 0.0125 0.6567 0.119 Uiso 1 1 calc R . . H39C H 0.3205 0.0248 0.5682 0.119 Uiso 1 1 calc R . . C20 C 0.2967(3) 0.1599(3) -0.0383(3) 0.0769(12) Uani 1 1 d . . . H20A H 0.2931 0.1571 0.0195 0.115 Uiso 1 1 calc R . . H20B H 0.2464 0.1371 -0.0574 0.115 Uiso 1 1 calc R . . H20C H 0.2958 0.2207 -0.0560 0.115 Uiso 1 1 calc R . . C80 C 1.1521(4) 0.4630(3) 0.4583(3) 0.0938(17) Uani 1 1 d . . . H80A H 1.1057 0.4326 0.4835 0.141 Uiso 1 1 calc R . . H80B H 1.1894 0.4782 0.4983 0.141 Uiso 1 1 calc R . . H80C H 1.1882 0.4248 0.4194 0.141 Uiso 1 1 calc R . . C64 C 0.5973(3) 0.7352(3) 0.2916(3) 0.0847(14) Uani 1 1 d . . . H64 H 0.5510 0.7793 0.3102 0.102 Uiso 1 1 calc R . . C74 C 0.9622(2) 0.4582(2) 0.2920(2) 0.0511(8) Uani 1 1 d . . . H74 H 0.9508 0.4035 0.2749 0.061 Uiso 1 1 calc R . . C30 C 0.4047(3) 0.5918(3) 0.4366(3) 0.0791(14) Uani 1 1 d . . . H30 H 0.3875 0.6471 0.4604 0.095 Uiso 1 1 calc R . . C65 C 0.6092(3) 0.7164(3) 0.2127(3) 0.0835(14) Uani 1 1 d . . . H65 H 0.5699 0.7461 0.1771 0.100 Uiso 1 1 calc R . . C79 C 1.1314(4) 0.6228(3) 0.4469(3) 0.0958(18) Uani 1 1 d . . . H79A H 1.1400 0.6621 0.4019 0.144 Uiso 1 1 calc R . . H79B H 1.1850 0.6123 0.4753 0.144 Uiso 1 1 calc R . . H79C H 1.0819 0.6495 0.4824 0.144 Uiso 1 1 calc R . . C5 C 0.7149(4) 0.3648(3) -0.1882(3) 0.0869(14) Uani 1 1 d . . . H5 H 0.6704 0.3927 -0.2199 0.104 Uiso 1 1 calc R . . C63 C 0.6523(3) 0.6903(3) 0.3439(3) 0.0796(13) Uani 1 1 d . . . H63 H 0.6429 0.7023 0.3986 0.096 Uiso 1 1 calc R . . C29 C 0.3880(4) 0.5173(3) 0.4760(3) 0.0873(15) Uani 1 1 d . . . H29 H 0.3604 0.5210 0.5280 0.105 Uiso 1 1 calc R . . C25 C 0.2632(4) 0.3627(4) 0.1960(3) 0.103(2) Uani 1 1 d . . . H25 H 0.2161 0.4082 0.1869 0.124 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 0.04569(11) 0.04091(10) 0.04085(11) 0.00118(8) -0.00680(8) -0.00458(8) I1 0.04022(10) 0.03552(9) 0.04306(11) -0.00247(7) -0.00096(7) -0.00598(7) I4 0.04990(11) 0.03792(9) 0.03357(10) -0.00217(7) -0.00121(8) -0.00351(8) I3 0.03773(10) 0.04218(10) 0.03812(10) -0.00020(8) 0.00373(7) -0.00605(8) Cu2 0.0450(3) 0.0452(2) 0.0474(3) -0.0013(2) 0.0068(2) -0.0042(2) Cu3 0.0448(2) 0.0427(2) 0.0399(2) 0.00200(19) -0.00261(18) -0.00324(19) Cu1 0.0485(3) 0.0498(3) 0.0409(3) -0.0088(2) -0.00237(19) -0.0060(2) Cu4 0.0505(3) 0.0400(2) 0.0445(3) -0.00014(19) -0.0036(2) -0.0114(2) P4 0.0434(4) 0.0353(4) 0.0443(4) 0.0016(3) -0.0043(3) -0.0085(3) P3 0.0361(4) 0.0360(3) 0.0369(4) 0.0010(3) -0.0013(3) -0.0045(3) P2 0.0381(4) 0.0409(4) 0.0386(4) -0.0012(3) 0.0022(3) -0.0022(3) P1 0.0431(4) 0.0465(4) 0.0380(4) -0.0085(3) -0.0010(3) -0.0038(3) C58 0.0415(16) 0.0348(14) 0.0420(17) 0.0000(12) -0.0047(12) -0.0070(12) C56 0.0393(16) 0.0454(16) 0.0353(16) 0.0013(13) -0.0025(12) -0.0083(13) C55 0.0423(16) 0.0406(15) 0.0406(17) -0.0009(13) -0.0013(13) -0.0011(13) C54 0.0432(16) 0.0346(14) 0.0420(17) 0.0042(12) -0.0056(13) -0.0045(13) C53 0.0346(15) 0.0407(15) 0.0366(15) 0.0015(12) -0.0042(12) -0.0069(12) C8 0.0425(18) 0.0504(18) 0.057(2) -0.0062(16) 0.0049(15) -0.0063(15) C57 0.0462(17) 0.0403(15) 0.0445(18) 0.0066(13) -0.0053(13) -0.0108(14) C13 0.0488(18) 0.0473(17) 0.0378(17) -0.0066(13) -0.0017(13) -0.0073(14) C18 0.057(2) 0.0497(17) 0.0356(17) -0.0061(14) 0.0013(14) -0.0071(15) C38 0.0352(15) 0.0468(16) 0.0451(17) -0.0027(14) -0.0010(12) -0.0103(13) N2 0.0551(18) 0.0625(18) 0.0612(19) 0.0201(15) -0.0140(14) -0.0194(15) C73 0.0474(18) 0.0376(15) 0.0492(19) -0.0011(14) -0.0044(14) -0.0077(14) C33 0.0379(16) 0.0432(15) 0.0398(16) -0.0013(13) -0.0002(12) -0.0035(13) C21 0.0459(18) 0.0506(17) 0.0381(17) 0.0025(14) -0.0021(13) -0.0054(14) C47 0.0362(16) 0.0359(14) 0.056(2) 0.0005(13) -0.0044(13) -0.0030(12) C1 0.059(2) 0.0461(17) 0.0413(18) -0.0084(14) 0.0010(15) -0.0049(15) N1 0.0585(19) 0.069(2) 0.066(2) -0.0167(16) -0.0084(15) -0.0226(16) N3 0.0647(19) 0.0523(16) 0.0430(16) 0.0042(13) 0.0097(13) -0.0080(14) C77 0.065(2) 0.0391(16) 0.061(2) -0.0017(15) -0.0151(17) -0.0127(16) C41 0.0411(16) 0.0383(15) 0.0382(16) 0.0029(12) -0.0004(12) -0.0032(13) C67 0.0409(17) 0.0442(16) 0.0520(19) 0.0085(14) -0.0038(14) -0.0053(14) C16 0.055(2) 0.0527(18) 0.0399(17) -0.0026(14) -0.0028(14) -0.0189(16) C36 0.0470(18) 0.0438(16) 0.0444(18) 0.0038(14) -0.0055(14) -0.0114(14) C17 0.066(2) 0.0485(18) 0.0428(18) -0.0081(15) -0.0003(15) -0.0178(17) C34 0.0379(17) 0.060(2) 0.0446(18) 0.0059(15) -0.0051(13) -0.0043(15) C27 0.0373(16) 0.0475(17) 0.0475(18) -0.0085(14) -0.0029(13) -0.0006(14) C52 0.0432(18) 0.0480(17) 0.061(2) -0.0075(16) -0.0083(15) -0.0041(15) C7 0.0439(17) 0.0474(17) 0.0480(19) -0.0092(15) 0.0028(14) -0.0048(14) C37 0.0399(16) 0.0479(17) 0.0485(18) 0.0051(14) -0.0120(13) -0.0058(14) C35 0.0383(17) 0.0583(19) 0.0505(19) 0.0058(16) -0.0018(14) -0.0139(15) C12 0.064(2) 0.061(2) 0.051(2) -0.0119(17) 0.0048(17) -0.0031(18) C76 0.056(2) 0.0486(18) 0.062(2) -0.0013(16) -0.0182(17) -0.0117(16) C61 0.0516(19) 0.0369(15) 0.059(2) 0.0001(15) -0.0011(15) -0.0079(14) C68 0.067(2) 0.056(2) 0.049(2) 0.0084(16) -0.0017(17) -0.0192(18) C10 0.053(2) 0.052(2) 0.091(3) -0.014(2) 0.017(2) 0.0015(18) C23 0.073(3) 0.061(2) 0.058(2) 0.0002(18) -0.0148(19) -0.012(2) C28 0.083(3) 0.061(2) 0.058(2) -0.0170(19) 0.018(2) -0.006(2) C22 0.058(2) 0.057(2) 0.056(2) -0.0015(17) -0.0130(17) -0.0060(17) C46 0.0480(19) 0.0495(18) 0.057(2) -0.0048(16) -0.0066(15) -0.0018(15) C59 0.080(3) 0.062(2) 0.044(2) 0.0032(17) 0.0133(18) -0.005(2) C45 0.050(2) 0.0509(19) 0.069(2) -0.0035(18) -0.0022(17) 0.0048(16) N4 0.092(3) 0.0530(18) 0.103(3) -0.0019(19) -0.053(2) -0.0126(18) C42 0.053(2) 0.0454(18) 0.068(2) -0.0076(17) -0.0154(17) 0.0009(15) C44 0.071(2) 0.0400(17) 0.053(2) -0.0042(15) 0.0012(17) -0.0005(17) C51 0.051(2) 0.052(2) 0.087(3) -0.0171(19) -0.0188(19) -0.0045(17) C15 0.051(2) 0.064(2) 0.065(2) -0.0223(19) -0.0008(17) -0.0132(18) C72 0.067(2) 0.055(2) 0.062(2) 0.0062(18) -0.0023(18) -0.0217(18) C14 0.054(2) 0.059(2) 0.061(2) -0.0248(18) -0.0042(17) -0.0121(17) C40 0.068(2) 0.056(2) 0.056(2) 0.0105(17) -0.0154(18) -0.0088(18) C2 0.058(2) 0.070(2) 0.058(2) -0.0018(19) 0.0058(17) -0.0094(19) C66 0.058(2) 0.064(2) 0.065(2) 0.0084(19) 0.0004(18) 0.0036(19) C48 0.0410(18) 0.0533(19) 0.070(2) 0.0161(18) 0.0012(16) -0.0050(15) C70 0.057(2) 0.089(3) 0.057(2) 0.026(2) -0.0063(18) -0.022(2) C75 0.060(2) 0.0399(17) 0.074(3) -0.0003(17) -0.0258(19) -0.0035(16) C71 0.070(3) 0.066(2) 0.076(3) 0.023(2) -0.006(2) -0.031(2) C50 0.042(2) 0.0403(18) 0.122(4) -0.006(2) -0.017(2) -0.0041(16) C32 0.070(2) 0.0479(19) 0.063(2) -0.0036(17) 0.0042(19) 0.0010(18) C78 0.060(2) 0.0371(16) 0.058(2) 0.0025(15) -0.0136(16) -0.0095(15) C11 0.066(2) 0.064(2) 0.068(3) -0.021(2) 0.016(2) -0.001(2) C9 0.050(2) 0.052(2) 0.081(3) 0.0016(19) 0.0028(19) -0.0053(17) C69 0.081(3) 0.081(3) 0.049(2) 0.007(2) -0.0069(19) -0.022(2) C60 0.079(3) 0.061(2) 0.046(2) 0.0136(17) 0.0057(18) -0.009(2) C49 0.041(2) 0.055(2) 0.108(4) 0.019(2) 0.003(2) -0.0090(17) C26 0.088(3) 0.062(2) 0.089(3) -0.014(2) -0.042(3) 0.014(2) C4 0.103(4) 0.054(2) 0.075(3) 0.008(2) 0.011(3) -0.011(2) C6 0.068(2) 0.060(2) 0.066(3) 0.0044(19) -0.0130(19) -0.0104(19) C24 0.072(3) 0.096(3) 0.067(3) -0.004(2) -0.032(2) -0.009(3) C62 0.065(2) 0.061(2) 0.063(2) -0.0070(19) 0.0033(19) -0.0024(19) C3 0.072(3) 0.065(2) 0.076(3) -0.006(2) 0.023(2) -0.012(2) C43 0.076(3) 0.0454(18) 0.073(3) -0.0129(18) -0.021(2) -0.0045(18) C31 0.079(3) 0.046(2) 0.100(4) -0.005(2) -0.009(3) -0.003(2) C19 0.075(3) 0.079(3) 0.063(2) -0.015(2) -0.006(2) -0.035(2) C39 0.066(3) 0.102(3) 0.078(3) 0.041(3) -0.016(2) -0.038(3) C20 0.058(2) 0.095(3) 0.084(3) -0.021(3) -0.006(2) -0.028(2) C80 0.102(4) 0.067(3) 0.122(4) 0.012(3) -0.066(3) -0.014(3) C64 0.077(3) 0.059(2) 0.110(4) -0.010(3) 0.018(3) 0.009(2) C74 0.052(2) 0.0369(16) 0.066(2) -0.0048(15) -0.0132(16) -0.0073(14) C30 0.075(3) 0.065(3) 0.094(4) -0.038(3) -0.014(2) 0.012(2) C65 0.070(3) 0.071(3) 0.101(4) 0.016(3) -0.003(3) 0.013(2) C79 0.106(4) 0.064(3) 0.126(5) -0.019(3) -0.064(4) -0.012(3) C5 0.108(4) 0.066(3) 0.088(3) 0.018(3) -0.026(3) -0.012(3) C63 0.085(3) 0.070(3) 0.080(3) -0.017(2) 0.009(2) -0.002(2) C29 0.102(4) 0.078(3) 0.075(3) -0.031(3) 0.016(3) 0.001(3) C25 0.103(4) 0.085(3) 0.120(5) -0.017(3) -0.072(4) 0.025(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 2.6552(5) . ? I2 Cu4 2.6637(5) . ? I2 Cu1 2.6679(5) . ? I1 Cu2 2.6715(5) . ? I1 Cu3 2.6945(5) . ? I1 Cu1 2.6991(5) . ? I4 Cu4 2.6729(5) . ? I4 Cu3 2.6755(5) . ? I4 Cu2 2.6930(5) . ? I3 Cu1 2.6800(5) . ? I3 Cu4 2.6842(5) . ? I3 Cu3 2.6884(5) . ? Cu2 P2 2.2509(9) . ? Cu2 Cu1 2.8779(7) . ? Cu2 Cu4 2.9610(7) . ? Cu3 P3 2.2525(9) . ? Cu1 P1 2.2522(9) . ? Cu1 Cu4 2.8505(7) . ? Cu4 P4 2.2509(8) . ? P4 C73 1.811(3) . ? P4 C67 1.830(3) . ? P4 C61 1.838(3) . ? P3 C53 1.820(3) . ? P3 C41 1.834(3) . ? P3 C47 1.839(3) . ? P2 C33 1.817(3) . ? P2 C27 1.825(3) . ? P2 C21 1.827(3) . ? P1 C13 1.814(3) . ? P1 C7 1.827(3) . ? P1 C1 1.834(4) . ? C58 C57 1.379(4) . ? C58 C53 1.394(4) . ? C56 N3 1.372(4) . ? C56 C55 1.406(4) . ? C56 C57 1.407(4) . ? C55 C54 1.382(4) . ? C54 C53 1.389(4) . ? C8 C7 1.381(5) . ? C8 C9 1.387(5) . ? C13 C18 1.385(4) . ? C13 C14 1.390(5) . ? C18 C17 1.371(5) . ? C38 C37 1.384(4) . ? C38 C33 1.392(4) . ? N2 C36 1.369(4) . ? N2 C40 1.445(4) . ? N2 C39 1.450(5) . ? C73 C74 1.388(4) . ? C73 C78 1.403(4) . ? C33 C34 1.389(4) . ? C21 C22 1.387(5) . ? C21 C26 1.381(5) . ? C47 C52 1.387(5) . ? C47 C48 1.398(5) . ? C1 C6 1.380(5) . ? C1 C2 1.391(5) . ? N1 C16 1.367(5) . ? N1 C20 1.437(5) . ? N1 C19 1.446(5) . ? N3 C60 1.440(4) . ? N3 C59 1.443(5) . ? C77 C78 1.371(5) . ? C77 C76 1.411(5) . ? C41 C46 1.385(4) . ? C41 C42 1.388(5) . ? C67 C68 1.374(5) . ? C67 C72 1.389(5) . ? C16 C15 1.408(5) . ? C16 C17 1.408(5) . ? C36 C35 1.412(5) . ? C36 C37 1.411(4) . ? C34 C35 1.378(5) . ? C27 C32 1.378(5) . ? C27 C28 1.383(5) . ? C52 C51 1.384(5) . ? C7 C12 1.393(5) . ? C12 C11 1.385(5) . ? C76 N4 1.367(5) . ? C76 C75 1.407(5) . ? C61 C62 1.386(5) . ? C61 C66 1.388(5) . ? C68 C69 1.397(5) . ? C10 C11 1.377(6) . ? C10 C9 1.377(6) . ? C23 C24 1.364(6) . ? C23 C22 1.375(5) . ? C28 C29 1.376(6) . ? C46 C45 1.386(5) . ? C45 C44 1.374(5) . ? N4 C79 1.433(5) . ? N4 C80 1.446(5) . ? C42 C43 1.384(5) . ? C44 C43 1.384(5) . ? C51 C50 1.365(6) . ? C15 C14 1.382(5) . ? C72 C71 1.385(5) . ? C2 C3 1.379(6) . ? C66 C65 1.388(6) . ? C48 C49 1.390(5) . ? C70 C71 1.368(6) . ? C70 C69 1.375(6) . ? C75 C74 1.381(5) . ? C50 C49 1.372(6) . ? C32 C31 1.395(5) . ? C26 C25 1.394(6) . ? C4 C5 1.361(7) . ? C4 C3 1.373(7) . ? C6 C5 1.390(6) . ? C24 C25 1.359(7) . ? C62 C63 1.380(6) . ? C31 C30 1.366(7) . ? C64 C63 1.377(7) . ? C64 C65 1.375(7) . ? C30 C29 1.368(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu2 I2 Cu4 67.656(15) . . ? Cu2 I2 Cu1 65.454(15) . . ? Cu4 I2 Cu1 64.640(15) . . ? Cu2 I1 Cu3 70.330(15) . . ? Cu2 I1 Cu1 64.801(15) . . ? Cu3 I1 Cu1 69.564(15) . . ? Cu4 I4 Cu3 70.444(14) . . ? Cu4 I4 Cu2 66.982(15) . . ? Cu3 I4 Cu2 70.292(15) . . ? Cu1 I3 Cu4 64.200(15) . . ? Cu1 I3 Cu3 69.938(15) . . ? Cu4 I3 Cu3 70.079(14) . . ? P2 Cu2 I2 115.48(3) . . ? P2 Cu2 I1 104.67(3) . . ? I2 Cu2 I1 111.688(18) . . ? P2 Cu2 I4 110.41(3) . . ? I2 Cu2 I4 107.807(17) . . ? I1 Cu2 I4 106.439(18) . . ? P2 Cu2 Cu1 145.55(3) . . ? I2 Cu2 Cu1 57.486(14) . . ? I1 Cu2 Cu1 58.063(14) . . ? I4 Cu2 Cu1 103.397(18) . . ? P2 Cu2 Cu4 150.73(3) . . ? I2 Cu2 Cu4 56.309(13) . . ? I1 Cu2 Cu4 104.238(18) . . ? I4 Cu2 Cu4 56.184(14) . . ? Cu1 Cu2 Cu4 58.424(16) . . ? P3 Cu3 I4 111.57(3) . . ? P3 Cu3 I3 113.58(3) . . ? I4 Cu3 I3 106.008(16) . . ? P3 Cu3 I1 113.12(3) . . ? I4 Cu3 I1 106.286(17) . . ? I3 Cu3 I1 105.684(17) . . ? P1 Cu1 I2 110.32(3) . . ? P1 Cu1 I3 108.64(3) . . ? I2 Cu1 I3 112.135(18) . . ? P1 Cu1 I1 109.40(3) . . ? I2 Cu1 I1 110.429(18) . . ? I3 Cu1 I1 105.791(17) . . ? P1 Cu1 Cu4 143.96(3) . . ? I2 Cu1 Cu4 57.608(14) . . ? I3 Cu1 Cu4 57.972(14) . . ? I1 Cu1 Cu4 106.558(18) . . ? P1 Cu1 Cu2 144.34(3) . . ? I2 Cu1 Cu2 57.060(14) . . ? I3 Cu1 Cu2 106.912(19) . . ? I1 Cu1 Cu2 57.136(14) . . ? Cu4 Cu1 Cu2 62.247(16) . . ? P4 Cu4 I2 109.59(3) . . ? P4 Cu4 I4 103.17(3) . . ? I2 Cu4 I4 108.153(17) . . ? P4 Cu4 I3 116.82(3) . . ? I2 Cu4 I3 112.134(17) . . ? I4 Cu4 I3 106.200(17) . . ? P4 Cu4 Cu1 151.94(3) . . ? I2 Cu4 Cu1 57.752(14) . . ? I4 Cu4 Cu1 104.659(18) . . ? I3 Cu4 Cu1 57.828(14) . . ? P4 Cu4 Cu2 138.20(3) . . ? I2 Cu4 Cu2 56.035(14) . . ? I4 Cu4 Cu2 56.834(14) . . ? I3 Cu4 Cu2 104.496(17) . . ? Cu1 Cu4 Cu2 59.329(16) . . ? C73 P4 C67 106.30(15) . . ? C73 P4 C61 103.33(16) . . ? C67 P4 C61 103.64(15) . . ? C73 P4 Cu4 116.11(10) . . ? C67 P4 Cu4 114.62(11) . . ? C61 P4 Cu4 111.53(11) . . ? C53 P3 C41 104.06(14) . . ? C53 P3 C47 102.99(14) . . ? C41 P3 C47 103.66(14) . . ? C53 P3 Cu3 114.11(10) . . ? C41 P3 Cu3 116.05(10) . . ? C47 P3 Cu3 114.43(10) . . ? C33 P2 C27 104.52(15) . . ? C33 P2 C21 101.39(15) . . ? C27 P2 C21 104.44(15) . . ? C33 P2 Cu2 117.17(10) . . ? C27 P2 Cu2 112.86(11) . . ? C21 P2 Cu2 114.93(11) . . ? C13 P1 C7 103.74(15) . . ? C13 P1 C1 104.61(16) . . ? C7 P1 C1 103.22(16) . . ? C13 P1 Cu1 113.62(11) . . ? C7 P1 Cu1 117.07(12) . . ? C1 P1 Cu1 113.18(11) . . ? C57 C58 C53 121.4(3) . . ? N3 C56 C55 121.2(3) . . ? N3 C56 C57 121.9(3) . . ? C55 C56 C57 117.0(3) . . ? C54 C55 C56 120.9(3) . . ? C55 C54 C53 121.9(3) . . ? C54 C53 C58 117.5(3) . . ? C54 C53 P3 118.2(2) . . ? C58 C53 P3 124.3(2) . . ? C7 C8 C9 121.3(3) . . ? C58 C57 C56 121.3(3) . . ? C18 C13 C14 116.7(3) . . ? C18 C13 P1 125.1(3) . . ? C14 C13 P1 118.2(2) . . ? C17 C18 C13 121.8(3) . . ? C37 C38 C33 121.8(3) . . ? C36 N2 C40 121.8(3) . . ? C36 N2 C39 120.4(3) . . ? C40 N2 C39 117.5(3) . . ? C74 C73 C78 116.5(3) . . ? C74 C73 P4 119.2(2) . . ? C78 C73 P4 124.3(3) . . ? C34 C33 C38 117.2(3) . . ? C34 C33 P2 122.6(2) . . ? C38 C33 P2 120.2(2) . . ? C22 C21 C26 117.3(3) . . ? C22 C21 P2 118.5(3) . . ? C26 C21 P2 124.1(3) . . ? C52 C47 C48 118.6(3) . . ? C52 C47 P3 122.9(3) . . ? C48 C47 P3 118.4(3) . . ? C6 C1 C2 118.4(4) . . ? C6 C1 P1 122.6(3) . . ? C2 C1 P1 118.9(3) . . ? C16 N1 C20 122.7(3) . . ? C16 N1 C19 119.9(3) . . ? C20 N1 C19 117.3(3) . . ? C56 N3 C60 121.1(3) . . ? C56 N3 C59 119.8(3) . . ? C60 N3 C59 118.5(3) . . ? C78 C77 C76 121.5(3) . . ? C46 C41 C42 118.8(3) . . ? C46 C41 P3 123.0(3) . . ? C42 C41 P3 118.2(2) . . ? C68 C67 C72 118.1(3) . . ? C68 C67 P4 118.5(3) . . ? C72 C67 P4 123.5(3) . . ? N1 C16 C15 121.6(3) . . ? N1 C16 C17 121.9(3) . . ? C15 C16 C17 116.5(3) . . ? N2 C36 C35 121.1(3) . . ? N2 C36 C37 122.3(3) . . ? C35 C36 C37 116.6(3) . . ? C18 C17 C16 121.9(3) . . ? C35 C34 C33 122.2(3) . . ? C32 C27 C28 118.9(3) . . ? C32 C27 P2 118.9(3) . . ? C28 C27 P2 122.1(3) . . ? C51 C52 C47 120.7(4) . . ? C8 C7 C12 118.4(3) . . ? C8 C7 P1 118.5(2) . . ? C12 C7 P1 123.0(3) . . ? C38 C37 C36 121.1(3) . . ? C34 C35 C36 121.1(3) . . ? C11 C12 C7 120.1(4) . . ? N4 C76 C75 121.9(3) . . ? N4 C76 C77 121.6(3) . . ? C75 C76 C77 116.5(3) . . ? C62 C61 C66 118.9(3) . . ? C62 C61 P4 120.6(3) . . ? C66 C61 P4 120.3(3) . . ? C67 C68 C69 121.6(4) . . ? C11 C10 C9 119.5(4) . . ? C24 C23 C22 120.6(4) . . ? C29 C28 C27 120.4(4) . . ? C23 C22 C21 121.4(4) . . ? C41 C46 C45 120.5(3) . . ? C44 C45 C46 120.9(3) . . ? C76 N4 C79 121.3(3) . . ? C76 N4 C80 120.4(3) . . ? C79 N4 C80 117.0(4) . . ? C43 C42 C41 120.2(3) . . ? C45 C44 C43 118.8(3) . . ? C50 C51 C52 120.4(4) . . ? C14 C15 C16 120.3(4) . . ? C71 C72 C67 120.7(4) . . ? C15 C14 C13 122.8(3) . . ? C3 C2 C1 120.9(4) . . ? C65 C66 C61 120.2(4) . . ? C49 C48 C47 119.7(4) . . ? C71 C70 C69 120.3(4) . . ? C74 C75 C76 121.0(3) . . ? C70 C71 C72 120.3(4) . . ? C51 C50 C49 120.0(4) . . ? C27 C32 C31 120.1(4) . . ? C77 C78 C73 122.0(3) . . ? C10 C11 C12 120.8(4) . . ? C10 C9 C8 119.9(4) . . ? C70 C69 C68 119.0(4) . . ? C50 C49 C48 120.6(4) . . ? C21 C26 C25 120.8(4) . . ? C5 C4 C3 119.7(4) . . ? C1 C6 C5 120.1(4) . . ? C25 C24 C23 119.3(4) . . ? C63 C62 C61 120.8(4) . . ? C4 C3 C2 120.0(4) . . ? C42 C43 C44 120.9(4) . . ? C30 C31 C32 120.4(4) . . ? C63 C64 C65 120.2(4) . . ? C73 C74 C75 122.4(3) . . ? C31 C30 C29 119.4(4) . . ? C64 C65 C66 120.0(5) . . ? C4 C5 C6 120.9(5) . . ? C64 C63 C62 119.8(5) . . ? C30 C29 C28 120.8(4) . . ? C24 C25 C26 120.6(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.60 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.461 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.060 _database_code_depnum_ccdc_archive 'CCDC 915491' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form ###END data_1\230K #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 4(C20H20N1P1Cu1I1) _chemical_formula_sum 'C80 H80 Cu4 I4 N4 P4' _chemical_formula_weight 1983.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.4242(3) _cell_length_b 15.5207(4) _cell_length_c 17.0532(4) _cell_angle_alpha 88.460(2) _cell_angle_beta 85.455(2) _cell_angle_gamma 81.274(2) _cell_volume 4022.04(16) _cell_formula_units_Z 2 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 21667 _cell_measurement_theta_min 2.5974 _cell_measurement_theta_max 74.0362 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2653 _exptl_crystal_size_mid 0.2031 _exptl_crystal_size_min 0.1483 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 14.328 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.117 _exptl_absorpt_correction_T_max 0.377 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 230(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5992 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43334 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 66.60 _reflns_number_total 14223 _reflns_number_gt 12123 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _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^)+(0.0299P)^2^+1.6827P] 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 14223 _refine_ls_number_parameters 873 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 I1 I 0.671207(15) 0.144571(14) 0.230865(14) 0.04445(6) Uani 1 1 d . . . I2 I 0.633460(16) 0.407684(15) 0.124204(14) 0.04779(6) Uani 1 1 d . . . I4 I 0.737774(16) 0.362136(14) 0.351700(13) 0.04561(6) Uani 1 1 d . . . I3 I 0.898857(15) 0.259063(15) 0.149622(13) 0.04452(6) Uani 1 1 d . . . Cu2 Cu 0.62227(4) 0.31473(4) 0.25678(3) 0.05241(14) Uani 1 1 d . . . Cu3 Cu 0.80730(4) 0.21282(4) 0.28090(3) 0.04830(13) Uani 1 1 d . . . Cu1 Cu 0.73248(4) 0.25098(4) 0.11881(3) 0.05242(14) Uani 1 1 d . . . Cu4 Cu 0.77978(4) 0.39480(3) 0.19965(3) 0.05014(13) Uani 1 1 d . . . P4 P 0.82574(6) 0.52559(6) 0.20113(6) 0.0462(2) Uani 1 1 d . . . P3 P 0.88879(6) 0.12233(6) 0.36155(5) 0.04101(19) Uani 1 1 d . . . P1 P 0.73326(6) 0.19195(6) -0.00044(6) 0.0477(2) Uani 1 1 d . . . P2 P 0.48709(6) 0.32507(6) 0.31948(6) 0.0451(2) Uani 1 1 d . . . C13 C 0.6290(3) 0.1603(3) -0.0201(2) 0.0487(9) Uani 1 1 d . . . C53 C 0.8320(2) 0.1020(2) 0.4566(2) 0.0417(8) Uani 1 1 d . . . C56 C 0.7482(2) 0.0818(2) 0.6084(2) 0.0445(8) Uani 1 1 d . . . C54 C 0.8316(2) 0.0201(2) 0.4912(2) 0.0444(8) Uani 1 1 d . . . H54 H 0.8600 -0.0293 0.4638 0.053 Uiso 1 1 calc R . . C21 C 0.3995(2) 0.3133(3) 0.2567(2) 0.0482(8) Uani 1 1 d . . . C2 C 0.8409(3) 0.0405(3) 0.0403(3) 0.0547(10) Uani 1 1 d . . . H2 H 0.8219 0.0574 0.0921 0.066 Uiso 1 1 calc R . . C34 C 0.5408(2) 0.2080(2) 0.4395(2) 0.0464(8) Uani 1 1 d . . . H34 H 0.5972 0.2222 0.4261 0.056 Uiso 1 1 calc R . . C58 C 0.7884(2) 0.1738(2) 0.4983(2) 0.0445(8) Uani 1 1 d . . . H58 H 0.7865 0.2298 0.4755 0.053 Uiso 1 1 calc R . . C73 C 0.9123(3) 0.5339(2) 0.2650(2) 0.0488(9) Uani 1 1 d . . . C36 C 0.4463(3) 0.1262(3) 0.5236(2) 0.0505(9) Uani 1 1 d . . . C47 C 0.9306(2) 0.0129(2) 0.3241(2) 0.0447(8) Uani 1 1 d . . . N3 N 0.7078(2) 0.0721(2) 0.6824(2) 0.0619(9) Uani 1 1 d . . . C57 C 0.7477(2) 0.1643(2) 0.5728(2) 0.0468(8) Uani 1 1 d . . . H57 H 0.7194 0.2139 0.5998 0.056 Uiso 1 1 calc R . . C62 C 0.8626(3) 0.5158(3) 0.0403(3) 0.0626(11) Uani 1 1 d . . . H62 H 0.8425 0.4617 0.0470 0.075 Uiso 1 1 calc R . . C55 C 0.7904(2) 0.0098(2) 0.5647(2) 0.0474(8) Uani 1 1 d . . . H55 H 0.7906 -0.0467 0.5862 0.057 Uiso 1 1 calc R . . C22 C 0.4006(3) 0.2337(3) 0.2212(3) 0.0649(11) Uani 1 1 d . . . H22 H 0.4471 0.1885 0.2291 0.078 Uiso 1 1 calc R . . N1 N 0.3782(3) 0.1087(3) -0.0692(2) 0.0701(10) Uani 1 1 d . . . N2 N 0.4335(2) 0.0685(3) 0.5841(2) 0.0670(10) Uani 1 1 d . . . C41 C 0.9885(2) 0.1625(2) 0.3887(2) 0.0498(9) Uani 1 1 d . . . C61 C 0.8625(3) 0.5674(3) 0.1050(2) 0.0518(9) Uani 1 1 d . . . C7 C 0.7571(3) 0.2662(3) -0.0820(2) 0.0550(10) Uani 1 1 d . . . C33 C 0.4710(2) 0.2454(2) 0.3967(2) 0.0462(8) Uani 1 1 d . . . C1 C 0.8125(2) 0.0938(3) -0.0219(2) 0.0510(9) Uani 1 1 d . . . C18 C 0.6182(3) 0.0887(3) -0.0632(2) 0.0553(10) Uani 1 1 d . . . H18 H 0.6684 0.0509 -0.0825 0.066 Uiso 1 1 calc R . . C17 C 0.5371(3) 0.0710(3) -0.0788(2) 0.0583(10) Uani 1 1 d . . . H17 H 0.5332 0.0217 -0.1085 0.070 Uiso 1 1 calc R . . C16 C 0.4598(3) 0.1242(3) -0.0516(2) 0.0576(10) Uani 1 1 d . . . C38 C 0.3879(2) 0.2207(3) 0.4187(2) 0.0529(9) Uani 1 1 d . . . H38 H 0.3394 0.2441 0.3908 0.064 Uiso 1 1 calc R . . C27 C 0.4516(2) 0.4301(3) 0.3660(2) 0.0509(9) Uani 1 1 d . . . C35 C 0.5287(3) 0.1502(3) 0.5015(2) 0.0518(9) Uani 1 1 d . . . H35 H 0.5772 0.1266 0.5294 0.062 Uiso 1 1 calc R . . C37 C 0.3764(2) 0.1635(3) 0.4797(2) 0.0548(10) Uani 1 1 d . . . H37 H 0.3201 0.1488 0.4927 0.066 Uiso 1 1 calc R . . C74 C 0.9622(3) 0.4587(3) 0.2919(3) 0.0556(10) Uani 1 1 d . . . H74 H 0.9513 0.4045 0.2749 0.067 Uiso 1 1 calc R . . C67 C 0.7367(3) 0.6109(2) 0.2368(3) 0.0548(10) Uani 1 1 d . . . C77 C 0.9960(3) 0.6155(3) 0.3427(3) 0.0620(11) Uani 1 1 d . . . H77 H 1.0064 0.6699 0.3597 0.074 Uiso 1 1 calc R . . C23 C 0.3353(3) 0.2193(3) 0.1745(3) 0.0706(12) Uani 1 1 d . . . H23 H 0.3375 0.1644 0.1518 0.085 Uiso 1 1 calc R . . C52 C 1.0132(3) -0.0312(3) 0.3380(3) 0.0563(10) Uani 1 1 d . . . H52 H 1.0506 -0.0052 0.3678 0.068 Uiso 1 1 calc R . . C6 C 0.8431(3) 0.0682(3) -0.0979(3) 0.0686(12) Uani 1 1 d . . . H6 H 0.8252 0.1037 -0.1410 0.082 Uiso 1 1 calc R . . C75 C 1.0269(3) 0.4602(3) 0.3425(3) 0.0659(12) Uani 1 1 d . . . H75 H 1.0584 0.4072 0.3595 0.079 Uiso 1 1 calc R . . C76 C 1.0470(3) 0.5390(3) 0.3696(3) 0.0601(10) Uani 1 1 d . . . C46 C 1.0065(3) 0.1702(3) 0.4661(3) 0.0564(10) Uani 1 1 d . . . H46 H 0.9684 0.1520 0.5069 0.068 Uiso 1 1 calc R . . C51 C 1.0407(3) -0.1139(3) 0.3077(3) 0.0643(11) Uani 1 1 d . . . H51 H 1.0968 -0.1434 0.3172 0.077 Uiso 1 1 calc R . . C50 C 0.9875(3) -0.1531(3) 0.2643(3) 0.0659(12) Uani 1 1 d . . . H50 H 1.0069 -0.2088 0.2435 0.079 Uiso 1 1 calc R . . C60 C 0.6721(3) 0.1484(3) 0.7274(3) 0.0708(13) Uani 1 1 d . . . H60A H 0.7188 0.1816 0.7361 0.106 Uiso 1 1 calc R . . H60B H 0.6458 0.1307 0.7776 0.106 Uiso 1 1 calc R . . H60C H 0.6277 0.1842 0.6987 0.106 Uiso 1 1 calc R . . C48 C 0.8764(3) -0.0273(3) 0.2803(3) 0.0614(11) Uani 1 1 d . . . H48 H 0.8202 0.0017 0.2705 0.074 Uiso 1 1 calc R . . C3 C 0.8968(3) -0.0371(3) 0.0275(3) 0.0691(12) Uani 1 1 d . . . H3 H 0.9150 -0.0730 0.0703 0.083 Uiso 1 1 calc R . . C66 C 0.8906(3) 0.6470(3) 0.0925(3) 0.0711(12) Uani 1 1 d . . . H66 H 0.8905 0.6839 0.1353 0.085 Uiso 1 1 calc R . . N4 N 1.1112(3) 0.5420(3) 0.4196(3) 0.0882(14) Uani 1 1 d . . . C39 C 0.5049(3) 0.0282(3) 0.6285(3) 0.0692(12) Uani 1 1 d . . . H39A H 0.5547 0.0059 0.5926 0.104 Uiso 1 1 calc R . . H39B H 0.4863 -0.0194 0.6603 0.104 Uiso 1 1 calc R . . H39C H 0.5217 0.0710 0.6624 0.104 Uiso 1 1 calc R . . C42 C 1.0462(3) 0.1890(3) 0.3295(3) 0.0630(11) Uani 1 1 d . . . H42 H 1.0351 0.1848 0.2764 0.076 Uiso 1 1 calc R . . C45 C 1.0808(3) 0.2050(3) 0.4840(3) 0.0717(13) Uani 1 1 d . . . H45 H 1.0921 0.2108 0.5368 0.086 Uiso 1 1 calc R . . C28 C 0.4107(3) 0.4374(3) 0.4410(3) 0.0759(14) Uani 1 1 d . . . H28 H 0.3983 0.3871 0.4689 0.091 Uiso 1 1 calc R . . C15 C 0.4693(3) 0.1955(3) -0.0061(3) 0.0643(12) Uani 1 1 d . . . H15 H 0.4191 0.2327 0.0141 0.077 Uiso 1 1 calc R . . C8 C 0.8417(3) 0.2879(3) -0.0938(3) 0.0705(12) Uani 1 1 d . . . H8 H 0.8852 0.2629 -0.0609 0.085 Uiso 1 1 calc R . . C72 C 0.6791(3) 0.6541(3) 0.1852(3) 0.0720(13) Uani 1 1 d . . . H72 H 0.6869 0.6414 0.1313 0.086 Uiso 1 1 calc R . . C44 C 1.1369(3) 0.2304(3) 0.4254(4) 0.0778(15) Uani 1 1 d . . . H44 H 1.1869 0.2538 0.4376 0.093 Uiso 1 1 calc R . . C4 C 0.9258(3) -0.0616(3) -0.0485(3) 0.0745(14) Uani 1 1 d . . . H4 H 0.9635 -0.1145 -0.0575 0.089 Uiso 1 1 calc R . . C64 C 0.9197(3) 0.6215(4) -0.0445(3) 0.0762(14) Uani 1 1 d . . . H64 H 0.9392 0.6399 -0.0949 0.091 Uiso 1 1 calc R . . C78 C 0.9316(3) 0.6126(3) 0.2922(3) 0.0581(10) Uani 1 1 d . . . H78 H 0.8994 0.6652 0.2753 0.070 Uiso 1 1 calc R . . C14 C 0.5523(3) 0.2116(3) 0.0094(3) 0.0654(12) Uani 1 1 d . . . H14 H 0.5567 0.2591 0.0411 0.078 Uiso 1 1 calc R . . C59 C 0.7120(4) -0.0123(3) 0.7201(3) 0.0725(13) Uani 1 1 d . . . H59A H 0.6914 -0.0524 0.6858 0.109 Uiso 1 1 calc R . . H59B H 0.6751 -0.0075 0.7691 0.109 Uiso 1 1 calc R . . H59C H 0.7723 -0.0338 0.7310 0.109 Uiso 1 1 calc R . . C68 C 0.7210(3) 0.6275(3) 0.3163(3) 0.0740(13) Uani 1 1 d . . . H68 H 0.7575 0.5962 0.3522 0.089 Uiso 1 1 calc R . . C12 C 0.6945(4) 0.3061(3) -0.1292(3) 0.0745(13) Uani 1 1 d . . . H12 H 0.6365 0.2941 -0.1215 0.089 Uiso 1 1 calc R . . C32 C 0.4706(3) 0.5047(3) 0.3276(3) 0.0695(12) Uani 1 1 d . . . H32 H 0.5002 0.5010 0.2772 0.083 Uiso 1 1 calc R . . C65 C 0.9193(3) 0.6736(4) 0.0179(3) 0.0787(15) Uani 1 1 d . . . H65 H 0.9385 0.7281 0.0107 0.094 Uiso 1 1 calc R . . C5 C 0.8996(3) -0.0089(3) -0.1107(3) 0.0776(14) Uani 1 1 d . . . H5 H 0.9202 -0.0254 -0.1623 0.093 Uiso 1 1 calc R . . C43 C 1.1204(3) 0.2219(3) 0.3491(4) 0.0794(16) Uani 1 1 d . . . H43 H 1.1600 0.2385 0.3088 0.095 Uiso 1 1 calc R . . C49 C 0.9047(4) -0.1097(3) 0.2512(3) 0.0737(13) Uani 1 1 d . . . H49 H 0.8672 -0.1366 0.2221 0.088 Uiso 1 1 calc R . . C10 C 0.7992(5) 0.3831(4) -0.1997(4) 0.0903(17) Uani 1 1 d . . . H10 H 0.8133 0.4223 -0.2400 0.108 Uiso 1 1 calc R . . C9 C 0.8624(4) 0.3451(3) -0.1524(3) 0.0808(15) Uani 1 1 d . . . H9 H 0.9200 0.3584 -0.1601 0.097 Uiso 1 1 calc R . . C31 C 0.4463(4) 0.5860(3) 0.3629(4) 0.0864(16) Uani 1 1 d . . . H31 H 0.4586 0.6368 0.3358 0.104 Uiso 1 1 calc R . . C19 C 0.2993(3) 0.1597(4) -0.0383(3) 0.0847(16) Uani 1 1 d . . . H19A H 0.2938 0.1528 0.0185 0.127 Uiso 1 1 calc R . . H19B H 0.2494 0.1407 -0.0603 0.127 Uiso 1 1 calc R . . H19C H 0.3007 0.2206 -0.0519 0.127 Uiso 1 1 calc R . . C24 C 0.2679(4) 0.2838(4) 0.1613(3) 0.0850(16) Uani 1 1 d . . . H24 H 0.2241 0.2744 0.1286 0.102 Uiso 1 1 calc R . . C40 C 0.3466(4) 0.0516(4) 0.6101(3) 0.0925(19) Uani 1 1 d . . . H40A H 0.3083 0.1064 0.6200 0.139 Uiso 1 1 calc R . . H40B H 0.3491 0.0166 0.6581 0.139 Uiso 1 1 calc R . . H40C H 0.3238 0.0203 0.5697 0.139 Uiso 1 1 calc R . . C70 C 0.5985(4) 0.7349(4) 0.2921(4) 0.0941(18) Uani 1 1 d . . . H70 H 0.5535 0.7791 0.3105 0.113 Uiso 1 1 calc R . . C20 C 0.3712(4) 0.0395(4) -0.1224(3) 0.0804(15) Uani 1 1 d . . . H20A H 0.4021 0.0499 -0.1727 0.121 Uiso 1 1 calc R . . H20B H 0.3097 0.0381 -0.1297 0.121 Uiso 1 1 calc R . . H20C H 0.3971 -0.0159 -0.1005 0.121 Uiso 1 1 calc R . . C26 C 0.3295(4) 0.3773(4) 0.2442(3) 0.0912(18) Uani 1 1 d . . . H26 H 0.3254 0.4316 0.2684 0.109 Uiso 1 1 calc R . . C79 C 1.1514(4) 0.4630(4) 0.4578(4) 0.104(2) Uani 1 1 d . . . H79A H 1.1061 0.4351 0.4864 0.156 Uiso 1 1 calc R . . H79B H 1.1922 0.4774 0.4941 0.156 Uiso 1 1 calc R . . H79C H 1.1829 0.4236 0.4184 0.156 Uiso 1 1 calc R . . C63 C 0.8917(3) 0.5419(4) -0.0345(3) 0.0773(14) Uani 1 1 d . . . H63 H 0.8923 0.5055 -0.0778 0.093 Uiso 1 1 calc R . . C30 C 0.4048(4) 0.5915(4) 0.4364(4) 0.0890(17) Uani 1 1 d . . . H30 H 0.3880 0.6461 0.4601 0.107 Uiso 1 1 calc R . . C11 C 0.7162(5) 0.3639(4) -0.1883(4) 0.0966(18) Uani 1 1 d . . . H11 H 0.6729 0.3902 -0.2208 0.116 Uiso 1 1 calc R . . C80 C 1.1308(4) 0.6226(4) 0.4464(4) 0.109(2) Uani 1 1 d . . . H80A H 1.1417 0.6602 0.4015 0.163 Uiso 1 1 calc R . . H80B H 1.1827 0.6117 0.4759 0.163 Uiso 1 1 calc R . . H80C H 1.0814 0.6506 0.4799 0.163 Uiso 1 1 calc R . . C71 C 0.6099(4) 0.7161(4) 0.2134(4) 0.0916(17) Uani 1 1 d . . . H71 H 0.5707 0.7452 0.1785 0.110 Uiso 1 1 calc R . . C29 C 0.3880(4) 0.5179(4) 0.4752(4) 0.0997(19) Uani 1 1 d . . . H29 H 0.3604 0.5219 0.5264 0.120 Uiso 1 1 calc R . . C69 C 0.6520(4) 0.6899(4) 0.3435(4) 0.0899(17) Uani 1 1 d . . . H69 H 0.6422 0.7011 0.3976 0.108 Uiso 1 1 calc R . . C25 C 0.2647(5) 0.3621(4) 0.1959(4) 0.116(3) Uani 1 1 d . . . H25 H 0.2180 0.4068 0.1871 0.139 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.04561(12) 0.03942(11) 0.04818(13) -0.00259(9) -0.00136(9) -0.00669(9) I2 0.05168(13) 0.04559(12) 0.04594(13) 0.00158(10) -0.00785(10) -0.00505(10) I4 0.05595(14) 0.04196(11) 0.03769(12) -0.00243(9) -0.00176(9) -0.00406(10) I3 0.04238(12) 0.04716(12) 0.04280(12) 0.00000(9) 0.00405(9) -0.00668(9) Cu2 0.0500(3) 0.0508(3) 0.0539(3) -0.0010(3) 0.0072(2) -0.0049(2) Cu3 0.0504(3) 0.0478(3) 0.0451(3) 0.0026(2) -0.0031(2) -0.0033(2) Cu1 0.0545(3) 0.0563(3) 0.0462(3) -0.0096(3) -0.0030(2) -0.0064(3) Cu4 0.0570(3) 0.0450(3) 0.0501(3) 0.0003(2) -0.0042(2) -0.0133(2) P4 0.0507(5) 0.0391(4) 0.0501(5) 0.0023(4) -0.0061(4) -0.0098(4) P3 0.0406(5) 0.0408(4) 0.0409(5) 0.0015(4) -0.0021(3) -0.0047(4) P1 0.0475(5) 0.0520(5) 0.0428(5) -0.0082(4) -0.0014(4) -0.0045(4) P2 0.0446(5) 0.0451(5) 0.0432(5) -0.0019(4) 0.0025(4) -0.0022(4) C13 0.050(2) 0.054(2) 0.042(2) -0.0070(16) -0.0030(16) -0.0070(17) C53 0.0398(18) 0.0439(18) 0.0411(19) -0.0001(15) -0.0018(14) -0.0060(15) C56 0.0381(18) 0.054(2) 0.0424(19) 0.0029(16) -0.0057(14) -0.0081(16) C54 0.0420(19) 0.0411(18) 0.051(2) -0.0015(16) -0.0045(15) -0.0079(15) C21 0.044(2) 0.059(2) 0.041(2) 0.0033(17) -0.0028(15) -0.0062(17) C2 0.046(2) 0.055(2) 0.062(3) -0.0050(19) 0.0044(18) -0.0083(18) C34 0.0335(18) 0.056(2) 0.051(2) -0.0038(17) -0.0019(15) -0.0120(16) C58 0.050(2) 0.0374(17) 0.045(2) 0.0050(15) -0.0052(16) -0.0034(15) C73 0.052(2) 0.0414(18) 0.054(2) 0.0014(16) -0.0069(17) -0.0081(16) C36 0.051(2) 0.052(2) 0.050(2) 0.0041(17) -0.0056(17) -0.0143(18) C47 0.049(2) 0.0425(18) 0.0404(19) 0.0037(15) -0.0008(15) -0.0024(16) N3 0.074(2) 0.059(2) 0.048(2) 0.0049(16) 0.0103(17) -0.0031(18) C57 0.049(2) 0.0437(19) 0.044(2) -0.0016(16) 0.0013(16) 0.0013(16) C62 0.073(3) 0.063(3) 0.055(3) 0.008(2) -0.003(2) -0.022(2) C55 0.052(2) 0.0427(19) 0.048(2) 0.0062(16) -0.0065(16) -0.0103(16) C22 0.069(3) 0.062(3) 0.064(3) -0.002(2) -0.014(2) -0.004(2) N1 0.058(2) 0.079(3) 0.079(3) -0.016(2) -0.0107(19) -0.025(2) N2 0.064(2) 0.074(2) 0.067(2) 0.026(2) -0.0196(18) -0.0206(19) C41 0.046(2) 0.0377(18) 0.064(2) 0.0028(17) -0.0063(17) -0.0015(16) C61 0.047(2) 0.051(2) 0.057(2) 0.0082(18) -0.0064(17) -0.0053(17) C7 0.064(3) 0.053(2) 0.045(2) -0.0124(18) 0.0025(18) -0.0008(19) C33 0.0427(19) 0.050(2) 0.045(2) -0.0022(16) 0.0019(15) -0.0066(16) C1 0.044(2) 0.054(2) 0.054(2) -0.0091(18) 0.0011(16) -0.0034(17) C18 0.065(3) 0.053(2) 0.048(2) -0.0072(18) 0.0004(18) -0.0085(19) C17 0.078(3) 0.051(2) 0.049(2) -0.0096(18) -0.007(2) -0.018(2) C16 0.073(3) 0.057(2) 0.046(2) -0.0006(18) -0.0056(19) -0.020(2) C38 0.0364(19) 0.068(2) 0.054(2) 0.0077(19) -0.0057(16) -0.0064(18) C27 0.045(2) 0.051(2) 0.055(2) -0.0070(18) -0.0032(17) 0.0003(17) C35 0.050(2) 0.052(2) 0.053(2) 0.0038(18) -0.0129(17) -0.0063(18) C37 0.039(2) 0.069(3) 0.058(2) 0.009(2) -0.0015(17) -0.0145(18) C74 0.050(2) 0.044(2) 0.075(3) -0.0045(19) -0.0169(19) -0.0087(17) C67 0.061(2) 0.0415(19) 0.062(3) 0.0026(18) -0.0016(19) -0.0112(18) C77 0.074(3) 0.044(2) 0.072(3) -0.0023(19) -0.019(2) -0.014(2) C23 0.078(3) 0.075(3) 0.063(3) -0.001(2) -0.015(2) -0.020(3) C52 0.050(2) 0.055(2) 0.062(3) -0.0030(19) -0.0075(18) -0.0008(18) C6 0.068(3) 0.072(3) 0.061(3) -0.016(2) 0.007(2) -0.001(2) C75 0.068(3) 0.046(2) 0.085(3) 0.001(2) -0.026(2) -0.005(2) C76 0.056(2) 0.059(2) 0.069(3) -0.005(2) -0.018(2) -0.013(2) C46 0.048(2) 0.054(2) 0.068(3) -0.009(2) -0.0108(19) -0.0041(18) C51 0.051(2) 0.056(2) 0.081(3) -0.004(2) -0.004(2) 0.007(2) C50 0.080(3) 0.045(2) 0.068(3) -0.003(2) 0.003(2) 0.004(2) C60 0.085(3) 0.075(3) 0.049(2) -0.002(2) 0.015(2) -0.008(3) C48 0.058(2) 0.048(2) 0.077(3) -0.008(2) -0.017(2) 0.0024(19) C3 0.058(3) 0.059(3) 0.086(3) 0.005(2) 0.004(2) -0.002(2) C66 0.087(3) 0.063(3) 0.068(3) 0.006(2) -0.004(2) -0.025(2) N4 0.095(3) 0.062(2) 0.117(4) -0.002(2) -0.057(3) -0.013(2) C39 0.083(3) 0.064(3) 0.063(3) 0.012(2) -0.021(2) -0.012(2) C42 0.051(2) 0.060(2) 0.075(3) 0.021(2) -0.001(2) -0.006(2) C45 0.061(3) 0.060(3) 0.095(4) -0.020(3) -0.026(3) 0.000(2) C28 0.087(3) 0.067(3) 0.069(3) -0.020(2) 0.014(3) -0.003(3) C15 0.044(2) 0.072(3) 0.079(3) -0.026(2) -0.007(2) -0.011(2) C8 0.068(3) 0.079(3) 0.062(3) 0.003(2) 0.008(2) -0.012(2) C72 0.064(3) 0.075(3) 0.073(3) 0.010(2) -0.002(2) 0.000(2) C44 0.050(3) 0.045(2) 0.139(5) -0.004(3) -0.016(3) -0.005(2) C4 0.054(3) 0.060(3) 0.105(4) -0.013(3) 0.013(3) 0.000(2) C64 0.064(3) 0.102(4) 0.064(3) 0.029(3) -0.007(2) -0.025(3) C78 0.066(3) 0.044(2) 0.067(3) 0.0052(19) -0.014(2) -0.0121(19) C14 0.062(3) 0.066(3) 0.070(3) -0.029(2) -0.003(2) -0.013(2) C59 0.093(4) 0.067(3) 0.054(3) 0.012(2) 0.005(2) -0.010(3) C68 0.080(3) 0.068(3) 0.069(3) -0.007(2) 0.001(2) 0.001(2) C12 0.081(3) 0.066(3) 0.078(3) 0.009(3) -0.018(3) -0.013(3) C32 0.081(3) 0.051(2) 0.072(3) -0.002(2) 0.005(2) -0.002(2) C65 0.071(3) 0.083(3) 0.089(4) 0.027(3) -0.007(3) -0.038(3) C5 0.079(3) 0.076(3) 0.071(3) -0.026(3) 0.019(3) 0.000(3) C43 0.044(2) 0.065(3) 0.127(5) 0.024(3) 0.007(3) -0.011(2) C49 0.089(4) 0.052(2) 0.082(3) -0.014(2) -0.026(3) -0.006(2) C10 0.122(5) 0.062(3) 0.084(4) 0.009(3) 0.013(4) -0.014(3) C9 0.075(3) 0.075(3) 0.089(4) -0.005(3) 0.024(3) -0.016(3) C31 0.087(4) 0.051(3) 0.120(5) -0.005(3) -0.011(3) -0.004(3) C19 0.059(3) 0.107(4) 0.096(4) -0.019(3) -0.011(3) -0.034(3) C24 0.075(3) 0.106(4) 0.077(3) -0.009(3) -0.036(3) -0.008(3) C40 0.082(4) 0.112(4) 0.091(4) 0.051(4) -0.014(3) -0.043(3) C70 0.081(4) 0.066(3) 0.125(5) -0.007(3) 0.020(4) 0.007(3) C20 0.089(4) 0.090(4) 0.072(3) -0.018(3) -0.013(3) -0.039(3) C26 0.105(4) 0.069(3) 0.098(4) -0.015(3) -0.051(3) 0.017(3) C79 0.107(5) 0.080(4) 0.136(6) 0.008(4) -0.074(4) -0.015(3) C63 0.087(4) 0.091(4) 0.057(3) 0.010(3) -0.008(2) -0.026(3) C30 0.085(4) 0.075(4) 0.103(5) -0.043(3) -0.017(3) 0.012(3) C11 0.120(5) 0.078(4) 0.092(4) 0.021(3) -0.029(4) -0.011(4) C80 0.123(5) 0.077(3) 0.137(6) -0.020(4) -0.080(5) -0.011(3) C71 0.078(4) 0.078(4) 0.109(5) 0.016(3) -0.003(3) 0.013(3) C29 0.111(5) 0.087(4) 0.093(4) -0.037(3) 0.017(4) 0.001(4) C69 0.097(4) 0.080(4) 0.085(4) -0.020(3) 0.009(3) 0.005(3) C25 0.110(5) 0.099(4) 0.135(6) -0.027(4) -0.075(4) 0.031(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 I1 Cu2 2.6730(6) . ? I1 Cu3 2.6951(6) . ? I1 Cu1 2.7001(6) . ? I2 Cu2 2.6572(6) . ? I2 Cu4 2.6642(6) . ? I2 Cu1 2.6682(6) . ? I4 Cu4 2.6764(6) . ? I4 Cu3 2.6776(6) . ? I4 Cu2 2.6934(7) . ? I3 Cu1 2.6818(6) . ? I3 Cu4 2.6859(6) . ? I3 Cu3 2.6910(6) . ? Cu2 P2 2.2519(11) . ? Cu2 Cu1 2.8958(8) . ? Cu2 Cu4 2.9785(8) . ? Cu3 P3 2.2536(10) . ? Cu1 P1 2.2512(11) . ? Cu1 Cu4 2.8696(8) . ? Cu4 P4 2.2508(10) . ? P4 C73 1.810(4) . ? P4 C61 1.827(4) . ? P4 C67 1.835(4) . ? P3 C53 1.823(3) . ? P3 C47 1.836(4) . ? P3 C41 1.840(4) . ? P1 C13 1.809(4) . ? P1 C1 1.828(4) . ? P1 C7 1.832(4) . ? P2 C33 1.811(4) . ? P2 C27 1.821(4) . ? P2 C21 1.822(4) . ? C13 C18 1.388(5) . ? C13 C14 1.389(6) . ? C53 C54 1.386(5) . ? C53 C58 1.393(5) . ? C56 N3 1.376(5) . ? C56 C57 1.402(5) . ? C56 C55 1.405(5) . ? C54 C55 1.377(5) . ? C21 C26 1.377(6) . ? C21 C22 1.387(6) . ? C2 C1 1.385(6) . ? C2 C3 1.383(6) . ? C34 C35 1.388(5) . ? C34 C33 1.393(5) . ? C58 C57 1.385(5) . ? C73 C74 1.386(5) . ? C73 C78 1.399(5) . ? C36 N2 1.371(5) . ? C36 C35 1.399(5) . ? C36 C37 1.404(5) . ? C47 C52 1.386(5) . ? C47 C48 1.388(6) . ? N3 C59 1.439(5) . ? N3 C60 1.442(6) . ? C62 C61 1.380(6) . ? C62 C63 1.390(6) . ? C22 C23 1.379(6) . ? N1 C16 1.374(6) . ? N1 C19 1.421(6) . ? N1 C20 1.445(6) . ? N2 C40 1.438(6) . ? N2 C39 1.440(5) . ? C41 C46 1.383(6) . ? C41 C42 1.388(6) . ? C61 C66 1.376(6) . ? C7 C12 1.371(6) . ? C7 C8 1.395(6) . ? C33 C38 1.412(5) . ? C1 C6 1.392(6) . ? C18 C17 1.368(6) . ? C17 C16 1.397(6) . ? C16 C15 1.400(6) . ? C38 C37 1.368(5) . ? C27 C32 1.374(6) . ? C27 C28 1.380(6) . ? C74 C75 1.373(6) . ? C67 C68 1.382(6) . ? C67 C72 1.387(6) . ? C77 C78 1.372(6) . ? C77 C76 1.409(6) . ? C23 C24 1.357(7) . ? C52 C51 1.389(6) . ? C6 C5 1.381(7) . ? C75 C76 1.406(6) . ? C76 N4 1.362(6) . ? C46 C45 1.397(6) . ? C51 C50 1.365(7) . ? C50 C49 1.382(7) . ? C48 C49 1.378(6) . ? C3 C4 1.381(7) . ? C66 C65 1.386(7) . ? N4 C80 1.425(6) . ? N4 C79 1.450(6) . ? C42 C43 1.389(7) . ? C45 C44 1.360(7) . ? C28 C29 1.379(7) . ? C15 C14 1.387(6) . ? C8 C9 1.371(7) . ? C72 C71 1.389(7) . ? C44 C43 1.360(8) . ? C4 C5 1.371(7) . ? C64 C65 1.353(8) . ? C64 C63 1.370(7) . ? C68 C69 1.385(7) . ? C12 C11 1.387(7) . ? C32 C31 1.399(7) . ? C10 C11 1.355(9) . ? C10 C9 1.369(8) . ? C31 C30 1.361(8) . ? C24 C25 1.358(8) . ? C70 C69 1.358(8) . ? C70 C71 1.373(8) . ? C26 C25 1.396(7) . ? C30 C29 1.353(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu2 I1 Cu3 70.493(18) . . ? Cu2 I1 Cu1 65.222(18) . . ? Cu3 I1 Cu1 69.821(18) . . ? Cu2 I2 Cu4 68.073(18) . . ? Cu2 I2 Cu1 65.881(18) . . ? Cu4 I2 Cu1 65.114(18) . . ? Cu4 I4 Cu3 70.706(17) . . ? Cu4 I4 Cu2 67.377(17) . . ? Cu3 I4 Cu2 70.449(18) . . ? Cu1 I3 Cu4 64.634(18) . . ? Cu1 I3 Cu3 70.154(18) . . ? Cu4 I3 Cu3 70.360(17) . . ? P2 Cu2 I2 115.52(3) . . ? P2 Cu2 I1 105.00(3) . . ? I2 Cu2 I1 111.32(2) . . ? P2 Cu2 I4 110.69(3) . . ? I2 Cu2 I4 107.57(2) . . ? I1 Cu2 I4 106.40(2) . . ? P2 Cu2 Cu1 145.45(4) . . ? I2 Cu2 Cu1 57.242(17) . . ? I1 Cu2 Cu1 57.840(17) . . ? I4 Cu2 Cu1 103.26(2) . . ? P2 Cu2 Cu4 150.60(4) . . ? I2 Cu2 Cu4 56.074(16) . . ? I1 Cu2 Cu4 104.09(2) . . ? I4 Cu2 Cu4 56.039(16) . . ? Cu1 Cu2 Cu4 58.463(19) . . ? P3 Cu3 I4 111.67(3) . . ? P3 Cu3 I3 113.66(3) . . ? I4 Cu3 I3 105.83(2) . . ? P3 Cu3 I1 113.27(3) . . ? I4 Cu3 I1 106.22(2) . . ? I3 Cu3 I1 105.56(2) . . ? P1 Cu1 I2 110.53(3) . . ? P1 Cu1 I3 108.76(3) . . ? I2 Cu1 I3 111.81(2) . . ? P1 Cu1 I1 109.80(3) . . ? I2 Cu1 I1 110.14(2) . . ? I3 Cu1 I1 105.68(2) . . ? P1 Cu1 Cu4 143.75(4) . . ? I2 Cu1 Cu4 57.375(17) . . ? I3 Cu1 Cu4 57.752(17) . . ? I1 Cu1 Cu4 106.37(2) . . ? P1 Cu1 Cu2 144.53(4) . . ? I2 Cu1 Cu2 56.877(17) . . ? I3 Cu1 Cu2 106.61(2) . . ? I1 Cu1 Cu2 56.938(17) . . ? Cu4 Cu1 Cu2 62.21(2) . . ? P4 Cu4 I2 109.96(3) . . ? P4 Cu4 I4 103.36(3) . . ? I2 Cu4 I4 107.87(2) . . ? P4 Cu4 I3 117.05(3) . . ? I2 Cu4 I3 111.81(2) . . ? I4 Cu4 I3 106.01(2) . . ? P4 Cu4 Cu1 152.01(4) . . ? I2 Cu4 Cu1 57.511(17) . . ? I4 Cu4 Cu1 104.41(2) . . ? I3 Cu4 Cu1 57.615(17) . . ? P4 Cu4 Cu2 138.23(4) . . ? I2 Cu4 Cu2 55.853(17) . . ? I4 Cu4 Cu2 56.584(17) . . ? I3 Cu4 Cu2 104.22(2) . . ? Cu1 Cu4 Cu2 59.327(19) . . ? C73 P4 C61 106.03(18) . . ? C73 P4 C67 103.43(19) . . ? C61 P4 C67 103.47(18) . . ? C73 P4 Cu4 115.99(12) . . ? C61 P4 Cu4 115.07(14) . . ? C67 P4 Cu4 111.50(13) . . ? C53 P3 C47 103.97(16) . . ? C53 P3 C41 103.15(17) . . ? C47 P3 C41 103.39(17) . . ? C53 P3 Cu3 114.29(12) . . ? C47 P3 Cu3 116.21(12) . . ? C41 P3 Cu3 114.27(12) . . ? C13 P1 C1 103.66(18) . . ? C13 P1 C7 104.39(19) . . ? C1 P1 C7 103.26(18) . . ? C13 P1 Cu1 113.57(13) . . ? C1 P1 Cu1 117.12(14) . . ? C7 P1 Cu1 113.42(13) . . ? C33 P2 C27 104.66(18) . . ? C33 P2 C21 101.86(17) . . ? C27 P2 C21 104.20(18) . . ? C33 P2 Cu2 116.91(12) . . ? C27 P2 Cu2 112.91(13) . . ? C21 P2 Cu2 114.80(12) . . ? C18 C13 C14 116.0(4) . . ? C18 C13 P1 125.7(3) . . ? C14 C13 P1 118.3(3) . . ? C54 C53 C58 117.8(3) . . ? C54 C53 P3 124.4(3) . . ? C58 C53 P3 117.7(3) . . ? N3 C56 C57 121.2(3) . . ? N3 C56 C55 121.8(3) . . ? C57 C56 C55 117.0(3) . . ? C55 C54 C53 121.4(3) . . ? C26 C21 C22 117.0(4) . . ? C26 C21 P2 124.4(3) . . ? C22 C21 P2 118.5(3) . . ? C1 C2 C3 121.1(4) . . ? C35 C34 C33 121.4(3) . . ? C57 C58 C53 121.3(3) . . ? C74 C73 C78 116.1(4) . . ? C74 C73 P4 119.6(3) . . ? C78 C73 P4 124.3(3) . . ? N2 C36 C35 122.4(4) . . ? N2 C36 C37 121.0(4) . . ? C35 C36 C37 116.6(3) . . ? C52 C47 C48 118.9(4) . . ? C52 C47 P3 123.1(3) . . ? C48 C47 P3 118.1(3) . . ? C56 N3 C59 121.0(4) . . ? C56 N3 C60 119.5(4) . . ? C59 N3 C60 118.9(4) . . ? C58 C57 C56 121.1(3) . . ? C61 C62 C63 121.6(4) . . ? C54 C55 C56 121.4(3) . . ? C23 C22 C21 121.8(4) . . ? C16 N1 C19 122.3(4) . . ? C16 N1 C20 119.7(4) . . ? C19 N1 C20 118.0(4) . . ? C36 N2 C40 121.0(4) . . ? C36 N2 C39 121.6(4) . . ? C40 N2 C39 117.2(4) . . ? C46 C41 C42 118.7(4) . . ? C46 C41 P3 122.3(3) . . ? C42 C41 P3 119.0(3) . . ? C66 C61 C62 117.5(4) . . ? C66 C61 P4 124.4(4) . . ? C62 C61 P4 118.1(3) . . ? C12 C7 C8 117.9(4) . . ? C12 C7 P1 123.3(4) . . ? C8 C7 P1 118.6(3) . . ? C34 C33 C38 116.8(3) . . ? C34 C33 P2 120.6(3) . . ? C38 C33 P2 122.5(3) . . ? C2 C1 C6 118.3(4) . . ? C2 C1 P1 118.5(3) . . ? C6 C1 P1 123.2(3) . . ? C17 C18 C13 122.4(4) . . ? C18 C17 C16 121.7(4) . . ? N1 C16 C17 122.1(4) . . ? N1 C16 C15 121.2(4) . . ? C17 C16 C15 116.8(4) . . ? C37 C38 C33 121.5(4) . . ? C32 C27 C28 118.2(4) . . ? C32 C27 P2 119.3(3) . . ? C28 C27 P2 122.3(3) . . ? C34 C35 C36 121.7(4) . . ? C38 C37 C36 121.9(3) . . ? C75 C74 C73 122.6(4) . . ? C68 C67 C72 118.8(4) . . ? C68 C67 P4 120.6(3) . . ? C72 C67 P4 120.3(4) . . ? C78 C77 C76 121.7(4) . . ? C24 C23 C22 120.4(5) . . ? C47 C52 C51 119.9(4) . . ? C5 C6 C1 120.6(5) . . ? C74 C75 C76 121.6(4) . . ? N4 C76 C75 122.5(4) . . ? N4 C76 C77 121.6(4) . . ? C75 C76 C77 115.9(4) . . ? C41 C46 C45 120.4(4) . . ? C50 C51 C52 121.1(4) . . ? C51 C50 C49 119.0(4) . . ? C49 C48 C47 120.3(4) . . ? C4 C3 C2 119.6(5) . . ? C61 C66 C65 121.2(5) . . ? C76 N4 C80 121.8(4) . . ? C76 N4 C79 120.3(4) . . ? C80 N4 C79 117.1(4) . . ? C43 C42 C41 119.7(5) . . ? C44 C45 C46 120.3(5) . . ? C29 C28 C27 120.4(5) . . ? C14 C15 C16 120.4(4) . . ? C9 C8 C7 121.1(5) . . ? C67 C72 C71 119.8(5) . . ? C45 C44 C43 119.7(5) . . ? C5 C4 C3 120.1(4) . . ? C65 C64 C63 120.3(5) . . ? C77 C78 C73 122.2(4) . . ? C15 C14 C13 122.6(4) . . ? C67 C68 C69 120.6(5) . . ? C7 C12 C11 120.5(5) . . ? C27 C32 C31 120.6(5) . . ? C64 C65 C66 120.3(5) . . ? C4 C5 C6 120.3(5) . . ? C44 C43 C42 121.3(5) . . ? C48 C49 C50 120.7(4) . . ? C11 C10 C9 119.8(5) . . ? C8 C9 C10 120.0(5) . . ? C30 C31 C32 119.9(5) . . ? C23 C24 C25 119.1(5) . . ? C69 C70 C71 120.2(5) . . ? C21 C26 C25 120.5(5) . . ? C64 C63 C62 119.2(5) . . ? C29 C30 C31 119.6(5) . . ? C10 C11 C12 120.8(6) . . ? C70 C71 C72 120.2(6) . . ? C30 C29 C28 121.1(6) . . ? C70 C69 C68 120.2(6) . . ? C24 C25 C26 121.1(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 66.60 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.555 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.063 _database_code_depnum_ccdc_archive 'CCDC 915492' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # end Validation Reply Form ###END data_1\260K #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 4(C20H20N1P1Cu1I1) _chemical_formula_sum 'C80 H80 Cu4 I4 N4 P4' _chemical_formula_weight 1983.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.4577(3) _cell_length_b 15.5354(4) _cell_length_c 17.0827(4) _cell_angle_alpha 88.465(2) _cell_angle_beta 85.427(2) _cell_angle_gamma 81.285(2) _cell_volume 4041.54(16) _cell_formula_units_Z 2 _cell_measurement_temperature 260(2) _cell_measurement_reflns_used 20664 _cell_measurement_theta_min 2.5930 _cell_measurement_theta_max 74.0068 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2653 _exptl_crystal_size_mid 0.2031 _exptl_crystal_size_min 0.1483 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 14.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.69592 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 260(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5992 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43410 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 66.60 _reflns_number_total 14282 _reflns_number_gt 11931 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _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^)+(0.0296P)^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 14282 _refine_ls_number_parameters 873 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0668 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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 I1 I 0.671431(14) 0.144581(13) 0.231055(13) 0.03473(6) Uani 1 1 d . . . I2 I 0.633757(15) 0.407024(15) 0.124713(13) 0.03863(6) Uani 1 1 d . . . I4 I 0.737878(15) 0.362003(14) 0.351598(12) 0.03598(6) Uani 1 1 d . . . I3 I 0.898508(14) 0.259167(14) 0.149692(13) 0.03501(6) Uani 1 1 d . . . Cu2 Cu 0.62203(4) 0.31447(4) 0.25739(3) 0.04394(14) Uani 1 1 d . . . Cu3 Cu 0.80742(3) 0.21267(3) 0.28104(3) 0.03940(12) Uani 1 1 d . . . Cu1 Cu 0.73265(4) 0.25052(4) 0.11866(3) 0.04418(13) Uani 1 1 d . . . Cu4 Cu 0.77996(4) 0.39510(3) 0.19969(3) 0.04165(13) Uani 1 1 d . . . P3 P 0.88874(6) 0.12237(5) 0.36145(5) 0.03078(18) Uani 1 1 d . . . P4 P 0.82566(6) 0.52582(6) 0.20131(6) 0.0365(2) Uani 1 1 d . . . P2 P 0.48706(6) 0.32508(6) 0.31981(5) 0.0350(2) Uani 1 1 d . . . P1 P 0.73336(6) 0.19174(6) -0.00056(5) 0.0383(2) Uani 1 1 d . . . C58 C 0.8323(2) 0.0206(2) 0.4908(2) 0.0351(8) Uani 1 1 d . . . H58 H 0.8610 -0.0281 0.4640 0.042 Uiso 1 1 calc R . . C53 C 0.8321(2) 0.1019(2) 0.45636(19) 0.0306(7) Uani 1 1 d . . . C8 C 0.8399(2) 0.0407(3) 0.0395(3) 0.0472(10) Uani 1 1 d . . . H8 H 0.8204 0.0571 0.0906 0.057 Uiso 1 1 calc R . . C41 C 0.9306(2) 0.0131(2) 0.3243(2) 0.0337(8) Uani 1 1 d . . . C34 C 0.5392(2) 0.2083(2) 0.4397(2) 0.0388(8) Uani 1 1 d . . . H34 H 0.5948 0.2227 0.4265 0.047 Uiso 1 1 calc R . . C56 C 0.7484(2) 0.0816(2) 0.6075(2) 0.0357(8) Uani 1 1 d . . . N1 N 0.3796(3) 0.1080(3) -0.0692(2) 0.0635(10) Uani 1 1 d . . . C54 C 0.7883(2) 0.1735(2) 0.4981(2) 0.0362(8) Uani 1 1 d . . . H54 H 0.7862 0.2288 0.4756 0.043 Uiso 1 1 calc R . . C13 C 0.6294(2) 0.1603(2) -0.0203(2) 0.0392(8) Uani 1 1 d . . . C55 C 0.7480(2) 0.1641(2) 0.5721(2) 0.0388(8) Uani 1 1 d . . . H55 H 0.7201 0.2132 0.5990 0.047 Uiso 1 1 calc R . . C33 C 0.4704(2) 0.2453(2) 0.3968(2) 0.0364(8) Uani 1 1 d . . . C27 C 0.3995(2) 0.3126(3) 0.2565(2) 0.0418(9) Uani 1 1 d . . . N3 N 0.7078(2) 0.0726(2) 0.68148(19) 0.0532(9) Uani 1 1 d . . . N2 N 0.4327(2) 0.0690(2) 0.5839(2) 0.0574(10) Uani 1 1 d . . . C21 C 0.4516(2) 0.4306(2) 0.3662(2) 0.0403(8) Uani 1 1 d . . . C57 C 0.7906(2) 0.0098(2) 0.5646(2) 0.0387(8) Uani 1 1 d . . . H57 H 0.7908 -0.0460 0.5859 0.046 Uiso 1 1 calc R . . C68 C 0.8623(3) 0.5163(3) 0.0409(2) 0.0577(11) Uani 1 1 d . . . H68 H 0.8425 0.4628 0.0474 0.069 Uiso 1 1 calc R . . C73 C 0.9120(2) 0.5343(2) 0.2656(2) 0.0408(9) Uani 1 1 d . . . C7 C 0.8124(2) 0.0939(3) -0.0223(2) 0.0428(9) Uani 1 1 d . . . C35 C 0.5282(2) 0.1509(3) 0.5012(2) 0.0423(9) Uani 1 1 d . . . H35 H 0.5763 0.1276 0.5285 0.051 Uiso 1 1 calc R . . C1 C 0.7577(3) 0.2658(3) -0.0815(2) 0.0451(9) Uani 1 1 d . . . C47 C 0.9881(2) 0.1627(2) 0.3886(2) 0.0393(8) Uani 1 1 d . . . C18 C 0.6191(3) 0.0887(3) -0.0634(2) 0.0452(9) Uani 1 1 d . . . H18 H 0.6689 0.0516 -0.0824 0.054 Uiso 1 1 calc R . . C74 C 0.9621(3) 0.4593(2) 0.2914(3) 0.0504(10) Uani 1 1 d . . . H74 H 0.9519 0.4059 0.2739 0.060 Uiso 1 1 calc R . . C36 C 0.4455(2) 0.1268(2) 0.5235(2) 0.0411(9) Uani 1 1 d . . . C17 C 0.5382(3) 0.0705(3) -0.0790(2) 0.0497(10) Uani 1 1 d . . . H17 H 0.5346 0.0214 -0.1079 0.060 Uiso 1 1 calc R . . C61 C 0.7364(3) 0.6110(2) 0.2368(3) 0.0473(10) Uani 1 1 d . . . C12 C 0.8440(3) 0.0689(3) -0.0981(3) 0.0584(12) Uani 1 1 d . . . H12 H 0.8277 0.1046 -0.1407 0.070 Uiso 1 1 calc R . . C16 C 0.4606(3) 0.1243(3) -0.0522(2) 0.0468(10) Uani 1 1 d . . . C77 C 0.9955(3) 0.6158(3) 0.3426(3) 0.0552(11) Uani 1 1 d . . . H77 H 1.0056 0.6694 0.3597 0.066 Uiso 1 1 calc R . . C38 C 0.3885(2) 0.2214(3) 0.4187(2) 0.0461(10) Uani 1 1 d . . . H38 H 0.3407 0.2453 0.3913 0.055 Uiso 1 1 calc R . . C67 C 0.8627(2) 0.5673(2) 0.1050(2) 0.0421(9) Uani 1 1 d . . . C37 C 0.3756(2) 0.1638(3) 0.4795(2) 0.0466(10) Uani 1 1 d . . . H37 H 0.3199 0.1490 0.4917 0.056 Uiso 1 1 calc R . . C42 C 1.0123(3) -0.0314(3) 0.3382(2) 0.0494(10) Uani 1 1 d . . . H42 H 1.0491 -0.0059 0.3679 0.059 Uiso 1 1 calc R . . C44 C 0.9876(3) -0.1528(3) 0.2646(3) 0.0564(11) Uani 1 1 d . . . H44 H 1.0071 -0.2078 0.2440 0.068 Uiso 1 1 calc R . . C52 C 1.0067(3) 0.1707(3) 0.4659(3) 0.0482(10) Uani 1 1 d . . . H52 H 0.9694 0.1530 0.5066 0.058 Uiso 1 1 calc R . . C39 C 0.5039(3) 0.0290(3) 0.6283(3) 0.0603(12) Uani 1 1 d . . . H39A H 0.5542 0.0096 0.5930 0.091 Uiso 1 1 calc R . . H39B H 0.4866 -0.0200 0.6577 0.091 Uiso 1 1 calc R . . H39C H 0.5184 0.0706 0.6637 0.091 Uiso 1 1 calc R . . C26 C 0.4106(3) 0.4373(3) 0.4410(3) 0.0693(14) Uani 1 1 d . . . H26 H 0.3986 0.3874 0.4684 0.083 Uiso 1 1 calc R . . C46 C 0.8767(3) -0.0266(3) 0.2804(3) 0.0544(11) Uani 1 1 d . . . H46 H 0.8215 0.0025 0.2703 0.065 Uiso 1 1 calc R . . C28 C 0.4010(3) 0.2338(3) 0.2217(3) 0.0570(11) Uani 1 1 d . . . H28 H 0.4466 0.1889 0.2301 0.068 Uiso 1 1 calc R . . C22 C 0.4707(3) 0.5048(3) 0.3277(3) 0.0620(12) Uani 1 1 d . . . H22 H 0.5004 0.5013 0.2781 0.074 Uiso 1 1 calc R . . C29 C 0.3364(3) 0.2198(3) 0.1746(3) 0.0653(13) Uani 1 1 d . . . H29 H 0.3389 0.1657 0.1517 0.078 Uiso 1 1 calc R . . C76 C 1.0462(3) 0.5392(3) 0.3690(3) 0.0528(10) Uani 1 1 d . . . C62 C 0.6794(3) 0.6533(3) 0.1852(3) 0.0676(13) Uani 1 1 d . . . H62 H 0.6873 0.6407 0.1319 0.081 Uiso 1 1 calc R . . C75 C 1.0269(3) 0.4607(3) 0.3424(3) 0.0606(12) Uani 1 1 d . . . H75 H 1.0582 0.4084 0.3592 0.073 Uiso 1 1 calc R . . C10 C 0.9252(3) -0.0617(3) -0.0491(3) 0.0707(15) Uani 1 1 d . . . H10 H 0.9619 -0.1142 -0.0582 0.085 Uiso 1 1 calc R . . C48 C 1.0455(3) 0.1886(3) 0.3289(3) 0.0566(11) Uani 1 1 d . . . H48 H 1.0341 0.1842 0.2767 0.068 Uiso 1 1 calc R . . C2 C 0.8411(3) 0.2875(3) -0.0930(3) 0.0652(13) Uani 1 1 d . . . H2 H 0.8842 0.2627 -0.0607 0.078 Uiso 1 1 calc R . . C3 C 0.8616(4) 0.3455(3) -0.1520(3) 0.0781(16) Uani 1 1 d . . . H3 H 0.9182 0.3594 -0.1590 0.094 Uiso 1 1 calc R . . C9 C 0.8964(3) -0.0370(3) 0.0266(3) 0.0605(12) Uani 1 1 d . . . H9 H 0.9147 -0.0722 0.0689 0.073 Uiso 1 1 calc R . . C43 C 1.0400(3) -0.1140(3) 0.3079(3) 0.0598(12) Uani 1 1 d . . . H43 H 1.0953 -0.1431 0.3176 0.072 Uiso 1 1 calc R . . C60 C 0.7118(3) -0.0120(3) 0.7197(3) 0.0656(13) Uani 1 1 d . . . H60A H 0.6913 -0.0518 0.6859 0.098 Uiso 1 1 calc R . . H60B H 0.6754 -0.0071 0.7680 0.098 Uiso 1 1 calc R . . H60C H 0.7713 -0.0334 0.7304 0.098 Uiso 1 1 calc R . . C59 C 0.6723(3) 0.1482(3) 0.7270(3) 0.0674(14) Uani 1 1 d . . . H59A H 0.7188 0.1797 0.7377 0.101 Uiso 1 1 calc R . . H59B H 0.6443 0.1304 0.7756 0.101 Uiso 1 1 calc R . . H59C H 0.6301 0.1851 0.6981 0.101 Uiso 1 1 calc R . . C51 C 1.0806(3) 0.2050(3) 0.4831(3) 0.0655(13) Uani 1 1 d . . . H51 H 1.0923 0.2107 0.5351 0.079 Uiso 1 1 calc R . . C78 C 0.9314(3) 0.6127(2) 0.2921(3) 0.0507(10) Uani 1 1 d . . . H78 H 0.8998 0.6647 0.2750 0.061 Uiso 1 1 calc R . . C15 C 0.4700(3) 0.1951(3) -0.0064(3) 0.0592(12) Uani 1 1 d . . . H15 H 0.4206 0.2320 0.0136 0.071 Uiso 1 1 calc R . . C14 C 0.5526(3) 0.2104(3) 0.0090(3) 0.0576(12) Uani 1 1 d . . . H14 H 0.5569 0.2569 0.0409 0.069 Uiso 1 1 calc R . . C6 C 0.6947(4) 0.3053(3) -0.1291(3) 0.0675(13) Uani 1 1 d . . . H6 H 0.6377 0.2926 -0.1219 0.081 Uiso 1 1 calc R . . C45 C 0.9049(3) -0.1099(3) 0.2512(3) 0.0672(14) Uani 1 1 d . . . H45 H 0.8680 -0.1366 0.2226 0.081 Uiso 1 1 calc R . . C20 C 0.2993(3) 0.1585(4) -0.0375(3) 0.0790(16) Uani 1 1 d . . . H20A H 0.2907 0.1459 0.0176 0.118 Uiso 1 1 calc R . . H20B H 0.2509 0.1441 -0.0639 0.118 Uiso 1 1 calc R . . H20C H 0.3028 0.2194 -0.0452 0.118 Uiso 1 1 calc R . . C70 C 0.9194(3) 0.6219(4) -0.0440(3) 0.0725(15) Uani 1 1 d . . . H70 H 0.9389 0.6401 -0.0937 0.087 Uiso 1 1 calc R . . C72 C 0.8906(3) 0.6472(3) 0.0929(3) 0.0660(13) Uani 1 1 d . . . H72 H 0.8901 0.6835 0.1354 0.079 Uiso 1 1 calc R . . C50 C 1.1360(3) 0.2304(3) 0.4242(4) 0.0729(16) Uani 1 1 d . . . H50 H 1.1850 0.2542 0.4362 0.087 Uiso 1 1 calc R . . C71 C 0.9191(3) 0.6745(4) 0.0191(3) 0.0751(15) Uani 1 1 d . . . H71 H 0.9381 0.7284 0.0123 0.090 Uiso 1 1 calc R . . C11 C 0.8995(3) -0.0086(3) -0.1103(3) 0.0702(14) Uani 1 1 d . . . H11 H 0.9198 -0.0249 -0.1613 0.084 Uiso 1 1 calc R . . C40 C 0.3458(3) 0.0517(4) 0.6095(3) 0.0863(19) Uani 1 1 d . . . H40A H 0.3078 0.1058 0.6194 0.129 Uiso 1 1 calc R . . H40B H 0.3481 0.0170 0.6568 0.129 Uiso 1 1 calc R . . H40C H 0.3236 0.0209 0.5694 0.129 Uiso 1 1 calc R . . C66 C 0.7211(3) 0.6274(3) 0.3162(3) 0.0686(13) Uani 1 1 d . . . H66 H 0.7573 0.5967 0.3516 0.082 Uiso 1 1 calc R . . C63 C 0.6097(4) 0.7154(4) 0.2137(4) 0.0892(19) Uani 1 1 d . . . H63 H 0.5711 0.7443 0.1791 0.107 Uiso 1 1 calc R . . C32 C 0.3308(4) 0.3765(3) 0.2438(3) 0.0859(19) Uani 1 1 d . . . H32 H 0.3272 0.4303 0.2674 0.103 Uiso 1 1 calc R . . C80 C 1.1511(4) 0.4631(4) 0.4566(4) 0.104(2) Uani 1 1 d . . . H80A H 1.1065 0.4308 0.4787 0.156 Uiso 1 1 calc R . . H80B H 1.1852 0.4777 0.4974 0.156 Uiso 1 1 calc R . . H80C H 1.1885 0.4282 0.4182 0.156 Uiso 1 1 calc R . . C30 C 0.2696(4) 0.2836(4) 0.1612(3) 0.0829(17) Uani 1 1 d . . . H30 H 0.2265 0.2740 0.1289 0.100 Uiso 1 1 calc R . . C19 C 0.3720(4) 0.0389(3) -0.1224(3) 0.0754(15) Uani 1 1 d . . . H19A H 0.4044 0.0478 -0.1715 0.113 Uiso 1 1 calc R . . H19B H 0.3113 0.0394 -0.1311 0.113 Uiso 1 1 calc R . . H19C H 0.3952 -0.0162 -0.0998 0.113 Uiso 1 1 calc R . . C69 C 0.8911(4) 0.5431(4) -0.0342(3) 0.0753(15) Uani 1 1 d . . . H69 H 0.8910 0.5074 -0.0771 0.090 Uiso 1 1 calc R . . C4 C 0.7990(5) 0.3827(4) -0.1999(4) 0.0859(18) Uani 1 1 d . . . H4 H 0.8130 0.4205 -0.2405 0.103 Uiso 1 1 calc R . . C64 C 0.5977(4) 0.7341(4) 0.2922(4) 0.094(2) Uani 1 1 d . . . H64 H 0.5526 0.7771 0.3104 0.112 Uiso 1 1 calc R . . C65 C 0.6517(4) 0.6897(4) 0.3433(4) 0.0887(18) Uani 1 1 d . . . H65 H 0.6423 0.7011 0.3968 0.106 Uiso 1 1 calc R . . C5 C 0.7159(5) 0.3637(4) -0.1875(4) 0.095(2) Uani 1 1 d . . . H5 H 0.6726 0.3905 -0.2187 0.114 Uiso 1 1 calc R . . C24 C 0.4047(4) 0.5912(4) 0.4362(4) 0.0831(18) Uani 1 1 d . . . H24 H 0.3887 0.6452 0.4596 0.100 Uiso 1 1 calc R . . C25 C 0.3873(4) 0.5174(4) 0.4750(4) 0.0929(19) Uani 1 1 d . . . H25 H 0.3592 0.5212 0.5252 0.111 Uiso 1 1 calc R . . C31 C 0.2659(4) 0.3616(4) 0.1952(4) 0.115(3) Uani 1 1 d . . . H31 H 0.2198 0.4058 0.1864 0.138 Uiso 1 1 calc R . . N4 N 1.1103(3) 0.5419(3) 0.4195(3) 0.0838(15) Uani 1 1 d . . . C79 C 1.1301(4) 0.6232(4) 0.4463(4) 0.107(2) Uani 1 1 d . . . H79A H 1.1403 0.6605 0.4019 0.160 Uiso 1 1 calc R . . H79B H 1.1816 0.6126 0.4750 0.160 Uiso 1 1 calc R . . H79C H 1.0815 0.6508 0.4797 0.160 Uiso 1 1 calc R . . C49 C 1.1202(3) 0.2212(3) 0.3479(4) 0.0743(16) Uani 1 1 d . . . H49 H 1.1597 0.2369 0.3080 0.089 Uiso 1 1 calc R . . C23 C 0.4457(4) 0.5851(3) 0.3626(4) 0.0805(16) Uani 1 1 d . . . H23 H 0.4571 0.6354 0.3355 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.03526(12) 0.02858(11) 0.04052(13) -0.00387(9) 0.00131(9) -0.00691(9) I2 0.04221(13) 0.03567(12) 0.03812(13) 0.00098(9) -0.00600(9) -0.00492(10) I4 0.04656(13) 0.03133(11) 0.02902(12) -0.00372(9) 0.00067(9) -0.00384(9) I3 0.03161(12) 0.03754(12) 0.03479(12) -0.00085(9) 0.00700(9) -0.00660(9) Cu2 0.0404(3) 0.0414(3) 0.0474(3) -0.0027(3) 0.0110(2) -0.0049(2) Cu3 0.0415(3) 0.0376(3) 0.0377(3) 0.0019(2) -0.0012(2) -0.0028(2) Cu1 0.0466(3) 0.0478(3) 0.0381(3) -0.0115(2) -0.0010(2) -0.0067(3) Cu4 0.0491(3) 0.0345(3) 0.0435(3) -0.0002(2) -0.0025(2) -0.0135(2) P3 0.0296(4) 0.0291(4) 0.0332(5) 0.0006(3) 0.0005(3) -0.0043(3) P4 0.0399(5) 0.0287(4) 0.0421(5) 0.0017(4) -0.0026(4) -0.0099(4) P2 0.0321(5) 0.0358(5) 0.0350(5) -0.0026(4) 0.0056(4) -0.0023(4) P1 0.0393(5) 0.0418(5) 0.0329(5) -0.0097(4) 0.0014(4) -0.0039(4) C58 0.0359(19) 0.0311(17) 0.039(2) -0.0027(15) -0.0027(15) -0.0077(15) C53 0.0271(17) 0.0311(17) 0.0333(18) 0.0028(14) -0.0007(13) -0.0049(14) C8 0.038(2) 0.046(2) 0.056(3) -0.0083(19) 0.0091(18) -0.0076(18) C41 0.0352(19) 0.0316(17) 0.0327(19) 0.0036(15) 0.0003(14) -0.0023(15) C34 0.0278(18) 0.046(2) 0.044(2) -0.0035(17) 0.0013(15) -0.0129(16) C56 0.0307(19) 0.042(2) 0.0340(19) 0.0013(16) -0.0003(14) -0.0058(16) N1 0.059(2) 0.070(3) 0.070(3) -0.018(2) -0.0102(19) -0.031(2) C54 0.041(2) 0.0288(17) 0.037(2) 0.0054(15) 0.0001(15) -0.0020(15) C13 0.041(2) 0.044(2) 0.034(2) -0.0076(16) 0.0008(15) -0.0101(17) C55 0.041(2) 0.0342(18) 0.039(2) -0.0027(16) 0.0009(16) -0.0010(16) C33 0.0327(19) 0.0401(19) 0.036(2) 0.0019(16) 0.0024(15) -0.0080(16) C27 0.039(2) 0.049(2) 0.036(2) 0.0050(17) -0.0009(16) -0.0053(18) N3 0.063(2) 0.051(2) 0.0406(19) 0.0043(16) 0.0150(16) -0.0038(18) N2 0.054(2) 0.064(2) 0.058(2) 0.0255(19) -0.0141(17) -0.0221(19) C21 0.033(2) 0.041(2) 0.045(2) -0.0084(17) -0.0025(16) 0.0002(16) C57 0.043(2) 0.0331(18) 0.042(2) 0.0076(16) -0.0017(16) -0.0123(16) C68 0.074(3) 0.055(3) 0.047(3) 0.010(2) -0.002(2) -0.021(2) C73 0.042(2) 0.0324(18) 0.050(2) 0.0019(17) -0.0067(17) -0.0093(16) C7 0.039(2) 0.043(2) 0.046(2) -0.0096(18) 0.0045(17) -0.0048(17) C35 0.035(2) 0.047(2) 0.046(2) 0.0052(18) -0.0084(16) -0.0086(17) C1 0.052(2) 0.044(2) 0.038(2) -0.0085(17) 0.0022(17) -0.0036(19) C47 0.0278(18) 0.0318(18) 0.058(2) 0.0029(17) -0.0012(16) -0.0038(15) C18 0.055(2) 0.043(2) 0.037(2) -0.0080(17) 0.0041(17) -0.0077(19) C74 0.053(3) 0.0314(19) 0.071(3) -0.0079(19) -0.017(2) -0.0102(18) C36 0.042(2) 0.044(2) 0.040(2) 0.0020(17) -0.0031(16) -0.0152(17) C17 0.067(3) 0.044(2) 0.043(2) -0.0143(18) -0.0025(19) -0.021(2) C61 0.050(2) 0.035(2) 0.058(3) 0.0012(18) 0.0015(19) -0.0131(18) C12 0.063(3) 0.062(3) 0.046(3) -0.013(2) 0.009(2) 0.001(2) C16 0.058(3) 0.049(2) 0.038(2) -0.0049(18) -0.0051(18) -0.023(2) C77 0.071(3) 0.035(2) 0.066(3) -0.0034(19) -0.018(2) -0.018(2) C38 0.031(2) 0.062(3) 0.045(2) 0.010(2) -0.0047(16) -0.0055(18) C67 0.037(2) 0.040(2) 0.050(2) 0.0114(18) -0.0025(17) -0.0082(17) C37 0.032(2) 0.063(3) 0.047(2) 0.008(2) -0.0004(16) -0.0171(19) C42 0.043(2) 0.047(2) 0.057(3) -0.005(2) -0.0045(19) -0.0019(19) C44 0.073(3) 0.033(2) 0.058(3) -0.0067(19) 0.005(2) 0.003(2) C52 0.038(2) 0.047(2) 0.060(3) -0.011(2) -0.0060(18) -0.0047(18) C39 0.075(3) 0.053(3) 0.056(3) 0.015(2) -0.021(2) -0.015(2) C26 0.082(4) 0.060(3) 0.060(3) -0.022(2) 0.021(3) -0.004(3) C46 0.050(3) 0.040(2) 0.073(3) -0.008(2) -0.016(2) 0.0016(19) C28 0.061(3) 0.051(2) 0.060(3) -0.002(2) -0.016(2) -0.004(2) C22 0.073(3) 0.040(2) 0.068(3) -0.005(2) 0.012(2) -0.004(2) C29 0.077(3) 0.069(3) 0.054(3) -0.009(2) -0.016(2) -0.018(3) C76 0.055(3) 0.046(2) 0.061(3) -0.005(2) -0.015(2) -0.013(2) C62 0.058(3) 0.069(3) 0.068(3) 0.008(3) 0.001(2) 0.009(3) C75 0.059(3) 0.038(2) 0.088(4) 0.000(2) -0.030(2) -0.003(2) C10 0.049(3) 0.049(3) 0.108(4) -0.020(3) 0.022(3) 0.002(2) C48 0.040(2) 0.052(2) 0.075(3) 0.018(2) 0.002(2) -0.005(2) C2 0.059(3) 0.072(3) 0.062(3) 0.005(3) 0.011(2) -0.011(2) C3 0.078(4) 0.068(3) 0.083(4) -0.003(3) 0.032(3) -0.013(3) C9 0.047(3) 0.050(3) 0.082(3) 0.003(2) 0.005(2) -0.004(2) C43 0.043(2) 0.051(3) 0.079(3) -0.004(2) 0.000(2) 0.010(2) C60 0.084(4) 0.060(3) 0.048(3) 0.013(2) 0.012(2) -0.008(3) C59 0.085(4) 0.072(3) 0.039(2) -0.002(2) 0.016(2) -0.006(3) C51 0.048(3) 0.051(3) 0.099(4) -0.025(3) -0.021(3) -0.003(2) C78 0.057(3) 0.0318(19) 0.066(3) 0.0033(19) -0.014(2) -0.0107(18) C15 0.044(2) 0.064(3) 0.071(3) -0.032(2) 0.000(2) -0.010(2) C14 0.045(2) 0.064(3) 0.067(3) -0.034(2) -0.001(2) -0.013(2) C6 0.075(3) 0.057(3) 0.072(3) 0.009(3) -0.015(3) -0.012(3) C45 0.081(4) 0.041(2) 0.084(4) -0.016(2) -0.026(3) -0.006(2) C20 0.051(3) 0.103(4) 0.090(4) -0.023(3) -0.005(3) -0.032(3) C70 0.058(3) 0.102(4) 0.059(3) 0.029(3) -0.002(2) -0.023(3) C72 0.077(3) 0.058(3) 0.068(3) 0.005(2) 0.000(3) -0.032(3) C50 0.038(3) 0.037(2) 0.145(6) -0.005(3) -0.017(3) -0.004(2) C71 0.071(3) 0.073(3) 0.088(4) 0.031(3) -0.002(3) -0.040(3) C11 0.066(3) 0.069(3) 0.069(3) -0.031(3) 0.023(3) 0.001(3) C40 0.073(4) 0.106(4) 0.089(4) 0.048(4) -0.015(3) -0.047(3) C66 0.075(3) 0.066(3) 0.061(3) -0.009(2) 0.002(2) 0.001(3) C63 0.073(4) 0.072(4) 0.110(5) 0.021(4) -0.001(3) 0.020(3) C32 0.094(4) 0.060(3) 0.105(4) -0.018(3) -0.057(4) 0.015(3) C80 0.111(5) 0.074(4) 0.138(6) 0.008(4) -0.081(5) -0.013(4) C30 0.081(4) 0.100(4) 0.072(4) -0.011(3) -0.040(3) -0.006(3) C19 0.085(4) 0.083(4) 0.069(3) -0.020(3) -0.009(3) -0.043(3) C69 0.086(4) 0.092(4) 0.051(3) 0.010(3) -0.003(3) -0.027(3) C4 0.119(5) 0.058(3) 0.077(4) 0.013(3) 0.015(4) -0.014(3) C64 0.084(4) 0.063(3) 0.123(6) -0.013(4) 0.026(4) 0.011(3) C65 0.095(4) 0.073(4) 0.090(4) -0.023(3) 0.012(3) 0.009(3) C5 0.118(5) 0.073(4) 0.096(5) 0.028(4) -0.028(4) -0.015(4) C24 0.076(4) 0.070(4) 0.099(5) -0.047(3) -0.017(3) 0.017(3) C25 0.108(5) 0.080(4) 0.083(4) -0.037(3) 0.016(3) 0.005(4) C31 0.109(5) 0.096(5) 0.139(6) -0.024(4) -0.086(5) 0.032(4) N4 0.095(3) 0.050(2) 0.117(4) -0.006(2) -0.061(3) -0.017(2) C79 0.118(5) 0.064(3) 0.151(6) -0.023(4) -0.079(5) -0.014(3) C49 0.035(3) 0.058(3) 0.127(5) 0.027(3) 0.005(3) -0.011(2) C23 0.084(4) 0.042(3) 0.113(5) -0.007(3) -0.007(3) -0.002(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 I1 Cu2 2.6739(6) . ? I1 Cu3 2.6972(6) . ? I1 Cu1 2.7025(6) . ? I2 Cu2 2.6601(6) . ? I2 Cu4 2.6655(6) . ? I2 Cu1 2.6685(6) . ? I4 Cu3 2.6792(6) . ? I4 Cu4 2.6799(6) . ? I4 Cu2 2.6955(6) . ? I3 Cu1 2.6827(6) . ? I3 Cu4 2.6873(6) . ? I3 Cu3 2.6938(6) . ? Cu2 P2 2.2511(10) . ? Cu2 Cu1 2.9142(8) . ? Cu2 Cu4 2.9962(8) . ? Cu3 P3 2.2524(10) . ? Cu1 P1 2.2527(10) . ? Cu1 Cu4 2.8848(8) . ? Cu4 P4 2.2504(10) . ? P3 C53 1.824(3) . ? P3 C41 1.834(3) . ? P3 C47 1.840(4) . ? P4 C73 1.816(4) . ? P4 C67 1.831(4) . ? P4 C61 1.838(4) . ? P2 C33 1.813(4) . ? P2 C21 1.828(4) . ? P2 C27 1.833(4) . ? P1 C13 1.809(4) . ? P1 C1 1.828(4) . ? P1 C7 1.827(4) . ? C58 C53 1.378(5) . ? C58 C57 1.388(5) . ? C53 C54 1.393(5) . ? C8 C7 1.377(6) . ? C8 C9 1.391(6) . ? C41 C42 1.379(5) . ? C41 C46 1.384(5) . ? C34 C35 1.377(5) . ? C34 C33 1.383(5) . ? C56 N3 1.378(5) . ? C56 C57 1.398(5) . ? C56 C55 1.403(5) . ? N1 C16 1.369(5) . ? N1 C20 1.439(6) . ? N1 C19 1.448(6) . ? C54 C55 1.378(5) . ? C13 C18 1.386(5) . ? C13 C14 1.383(5) . ? C33 C38 1.394(5) . ? C27 C28 1.372(6) . ? C27 C32 1.367(6) . ? N3 C59 1.440(6) . ? N3 C60 1.447(5) . ? N2 C36 1.372(5) . ? N2 C39 1.439(5) . ? N2 C40 1.441(6) . ? C21 C22 1.371(6) . ? C21 C26 1.380(6) . ? C68 C67 1.370(6) . ? C68 C69 1.397(6) . ? C73 C74 1.380(5) . ? C73 C78 1.393(5) . ? C7 C12 1.391(5) . ? C35 C36 1.406(5) . ? C1 C6 1.380(6) . ? C1 C2 1.378(6) . ? C47 C48 1.390(6) . ? C47 C52 1.387(5) . ? C18 C17 1.370(6) . ? C74 C75 1.381(6) . ? C36 C37 1.408(5) . ? C17 C16 1.406(6) . ? C61 C62 1.380(6) . ? C61 C66 1.382(6) . ? C12 C11 1.379(6) . ? C16 C15 1.399(5) . ? C77 C78 1.372(6) . ? C77 C76 1.406(6) . ? C38 C37 1.375(5) . ? C67 C72 1.380(6) . ? C42 C43 1.390(6) . ? C44 C43 1.354(6) . ? C44 C45 1.383(6) . ? C52 C51 1.385(6) . ? C26 C25 1.372(7) . ? C46 C45 1.394(6) . ? C28 C29 1.377(6) . ? C22 C23 1.384(7) . ? C29 C30 1.348(7) . ? C76 N4 1.371(5) . ? C76 C75 1.395(6) . ? C62 C63 1.399(7) . ? C10 C11 1.361(7) . ? C10 C9 1.378(7) . ? C48 C49 1.394(7) . ? C2 C3 1.384(7) . ? C3 C4 1.369(8) . ? C51 C50 1.358(7) . ? C15 C14 1.381(6) . ? C6 C5 1.384(7) . ? C70 C71 1.370(8) . ? C70 C69 1.363(7) . ? C72 C71 1.378(6) . ? C50 C49 1.360(7) . ? C66 C65 1.390(7) . ? C63 C64 1.372(8) . ? C32 C31 1.401(7) . ? C80 N4 1.444(6) . ? C30 C31 1.349(8) . ? C4 C5 1.359(8) . ? C64 C65 1.358(8) . ? C24 C23 1.360(8) . ? C24 C25 1.360(8) . ? N4 C79 1.438(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu2 I1 Cu3 70.683(17) . . ? Cu2 I1 Cu1 65.642(17) . . ? Cu3 I1 Cu1 70.006(17) . . ? Cu2 I2 Cu4 68.472(18) . . ? Cu2 I2 Cu1 66.310(18) . . ? Cu4 I2 Cu1 65.482(17) . . ? Cu3 I4 Cu4 70.905(17) . . ? Cu3 I4 Cu2 70.630(17) . . ? Cu4 I4 Cu2 67.750(17) . . ? Cu1 I3 Cu4 64.988(17) . . ? Cu1 I3 Cu3 70.353(18) . . ? Cu4 I3 Cu3 70.571(17) . . ? P2 Cu2 I2 115.57(3) . . ? P2 Cu2 I1 105.34(3) . . ? I2 Cu2 I1 110.96(2) . . ? P2 Cu2 I4 111.00(3) . . ? I2 Cu2 I4 107.32(2) . . ? I1 Cu2 I4 106.32(2) . . ? P2 Cu2 Cu1 145.41(4) . . ? I2 Cu2 Cu1 56.984(16) . . ? I1 Cu2 Cu1 57.652(17) . . ? I4 Cu2 Cu1 103.04(2) . . ? P2 Cu2 Cu4 150.49(4) . . ? I2 Cu2 Cu4 55.849(15) . . ? I1 Cu2 Cu4 103.89(2) . . ? I4 Cu2 Cu4 55.878(16) . . ? Cu1 Cu2 Cu4 58.411(18) . . ? P3 Cu3 I4 111.76(3) . . ? P3 Cu3 I3 113.78(3) . . ? I4 Cu3 I3 105.704(19) . . ? P3 Cu3 I1 113.36(3) . . ? I4 Cu3 I1 106.121(19) . . ? I3 Cu3 I1 105.457(19) . . ? P1 Cu1 I2 110.64(3) . . ? P1 Cu1 I3 108.97(3) . . ? I2 Cu1 I3 111.58(2) . . ? P1 Cu1 I1 110.09(3) . . ? I2 Cu1 I1 109.82(2) . . ? I3 Cu1 I1 105.62(2) . . ? P1 Cu1 Cu4 143.65(4) . . ? I2 Cu1 Cu4 57.208(16) . . ? I3 Cu1 Cu4 57.583(16) . . ? I1 Cu1 Cu4 106.19(2) . . ? P1 Cu1 Cu2 144.53(4) . . ? I2 Cu1 Cu2 56.706(16) . . ? I3 Cu1 Cu2 106.41(2) . . ? I1 Cu1 Cu2 56.706(16) . . ? Cu4 Cu1 Cu2 62.215(19) . . ? P4 Cu4 I2 110.27(3) . . ? P4 Cu4 I4 103.44(3) . . ? I2 Cu4 I4 107.61(2) . . ? P4 Cu4 I3 117.28(3) . . ? I2 Cu4 I3 111.53(2) . . ? I4 Cu4 I3 105.866(19) . . ? P4 Cu4 Cu1 152.11(4) . . ? I2 Cu4 Cu1 57.310(16) . . ? I4 Cu4 Cu1 104.22(2) . . ? I3 Cu4 Cu1 57.429(16) . . ? P4 Cu4 Cu2 138.16(3) . . ? I2 Cu4 Cu2 55.679(16) . . ? I4 Cu4 Cu2 56.372(16) . . ? I3 Cu4 Cu2 104.04(2) . . ? Cu1 Cu4 Cu2 59.374(19) . . ? C53 P3 C41 103.87(15) . . ? C53 P3 C47 103.07(17) . . ? C41 P3 C47 103.41(16) . . ? C53 P3 Cu3 114.32(11) . . ? C41 P3 Cu3 116.32(11) . . ? C47 P3 Cu3 114.26(12) . . ? C73 P4 C67 106.17(18) . . ? C73 P4 C61 103.47(19) . . ? C67 P4 C61 103.66(18) . . ? C73 P4 Cu4 115.98(12) . . ? C67 P4 Cu4 114.84(13) . . ? C61 P4 Cu4 111.42(13) . . ? C33 P2 C21 104.89(18) . . ? C33 P2 C27 101.50(17) . . ? C21 P2 C27 104.57(17) . . ? C33 P2 Cu2 116.95(12) . . ? C21 P2 Cu2 112.83(13) . . ? C27 P2 Cu2 114.64(12) . . ? C13 P1 C1 104.60(18) . . ? C13 P1 C7 103.68(18) . . ? C1 P1 C7 102.98(18) . . ? C13 P1 Cu1 113.65(12) . . ? C1 P1 Cu1 113.31(13) . . ? C7 P1 Cu1 117.19(13) . . ? C53 C58 C57 121.6(3) . . ? C58 C53 C54 117.7(3) . . ? C58 C53 P3 124.4(3) . . ? C54 C53 P3 117.8(3) . . ? C7 C8 C9 121.0(4) . . ? C42 C41 C46 118.6(4) . . ? C42 C41 P3 123.5(3) . . ? C46 C41 P3 117.8(3) . . ? C35 C34 C33 122.4(3) . . ? N3 C56 C57 122.0(3) . . ? N3 C56 C55 120.7(3) . . ? C57 C56 C55 117.4(3) . . ? C16 N1 C20 122.6(4) . . ? C16 N1 C19 120.3(4) . . ? C20 N1 C19 117.2(4) . . ? C55 C54 C53 121.5(3) . . ? C18 C13 C14 115.8(4) . . ? C18 C13 P1 125.3(3) . . ? C14 C13 P1 118.9(3) . . ? C54 C55 C56 120.9(3) . . ? C34 C33 C38 116.6(3) . . ? C34 C33 P2 120.7(3) . . ? C38 C33 P2 122.7(3) . . ? C28 C27 C32 117.6(4) . . ? C28 C27 P2 118.5(3) . . ? C32 C27 P2 123.8(3) . . ? C56 N3 C59 120.5(3) . . ? C56 N3 C60 120.7(3) . . ? C59 N3 C60 118.1(3) . . ? C36 N2 C39 121.6(4) . . ? C36 N2 C40 120.8(4) . . ? C39 N2 C40 117.4(4) . . ? C22 C21 C26 118.8(4) . . ? C22 C21 P2 119.4(3) . . ? C26 C21 P2 121.7(3) . . ? C58 C57 C56 120.9(3) . . ? C67 C68 C69 121.4(4) . . ? C74 C73 C78 116.5(4) . . ? C74 C73 P4 119.3(3) . . ? C78 C73 P4 124.2(3) . . ? C8 C7 C12 118.4(4) . . ? C8 C7 P1 118.2(3) . . ? C12 C7 P1 123.4(3) . . ? C34 C35 C36 121.1(3) . . ? C6 C1 C2 118.2(4) . . ? C6 C1 P1 122.7(3) . . ? C2 C1 P1 119.0(3) . . ? C48 C47 C52 118.7(4) . . ? C48 C47 P3 118.4(3) . . ? C52 C47 P3 122.9(3) . . ? C17 C18 C13 122.4(4) . . ? C73 C74 C75 122.5(4) . . ? N2 C36 C35 122.5(3) . . ? N2 C36 C37 120.9(3) . . ? C35 C36 C37 116.7(3) . . ? C18 C17 C16 121.5(4) . . ? C62 C61 C66 119.5(4) . . ? C62 C61 P4 120.1(3) . . ? C66 C61 P4 120.2(3) . . ? C11 C12 C7 120.2(4) . . ? N1 C16 C15 121.4(4) . . ? N1 C16 C17 121.9(4) . . ? C15 C16 C17 116.6(4) . . ? C78 C77 C76 121.2(4) . . ? C37 C38 C33 122.4(3) . . ? C68 C67 C72 117.8(4) . . ? C68 C67 P4 118.2(3) . . ? C72 C67 P4 124.0(4) . . ? C38 C37 C36 120.9(3) . . ? C41 C42 C43 120.5(4) . . ? C43 C44 C45 119.4(4) . . ? C51 C52 C47 120.5(4) . . ? C25 C26 C21 120.2(5) . . ? C41 C46 C45 120.3(4) . . ? C27 C28 C29 121.3(4) . . ? C21 C22 C23 120.1(5) . . ? C30 C29 C28 120.7(5) . . ? N4 C76 C75 121.8(4) . . ? N4 C76 C77 121.5(4) . . ? C75 C76 C77 116.7(4) . . ? C61 C62 C63 119.4(5) . . ? C76 C75 C74 121.0(4) . . ? C11 C10 C9 119.6(4) . . ? C47 C48 C49 119.6(5) . . ? C1 C2 C3 120.9(5) . . ? C4 C3 C2 120.3(5) . . ? C10 C9 C8 119.7(5) . . ? C44 C43 C42 121.0(4) . . ? C50 C51 C52 120.3(5) . . ? C77 C78 C73 122.0(4) . . ? C14 C15 C16 120.1(4) . . ? C13 C14 C15 123.5(4) . . ? C1 C6 C5 120.3(5) . . ? C44 C45 C46 120.2(4) . . ? C71 C70 C69 120.3(5) . . ? C71 C72 C67 121.5(5) . . ? C51 C50 C49 120.3(5) . . ? C70 C71 C72 119.8(5) . . ? C10 C11 C12 121.2(4) . . ? C65 C66 C61 120.3(5) . . ? C64 C63 C62 120.5(5) . . ? C27 C32 C31 120.5(5) . . ? C29 C30 C31 119.4(5) . . ? C70 C69 C68 119.3(5) . . ? C5 C4 C3 119.2(5) . . ? C65 C64 C63 120.0(5) . . ? C64 C65 C66 120.3(6) . . ? C4 C5 C6 121.1(6) . . ? C23 C24 C25 119.2(5) . . ? C24 C25 C26 120.9(6) . . ? C30 C31 C32 120.5(5) . . ? C76 N4 C79 121.4(4) . . ? C76 N4 C80 120.5(4) . . ? C79 N4 C80 117.5(4) . . ? C50 C49 C48 120.6(5) . . ? C24 C23 C22 120.7(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.60 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.624 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.072 # end Validation Reply Form ###END _database_code_depnum_ccdc_archive 'CCDC 915493' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_1c #TrackingRef '1c&1d.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 4(C20H20NPCuI) _chemical_formula_sum 'C80 H80 Cu4 I4 N4 P4' _chemical_formula_weight 1983.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.722(3) _cell_length_b 25.304(6) _cell_length_c 27.966(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.810(6) _cell_angle_gamma 90.00 _cell_volume 9596(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11564 _cell_measurement_theta_min 2.2993 _cell_measurement_theta_max 27.5126 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 2.265 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3972 _exptl_absorpt_correction_T_max 0.4644 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71682 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 21825 _reflns_number_gt 14306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1158P)^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 21825 _refine_ls_number_parameters 873 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.2097 _refine_ls_wR_factor_gt 0.1838 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.368544(13) 0.302281(7) 0.670550(7) 0.05678(5) Uani 1 1 d . . . I3 I 0.414352(12) 0.465408(7) 0.644061(7) 0.05565(5) Uani 1 1 d . . . I2 I 0.308151(14) 0.423227(7) 0.776048(7) 0.06126(5) Uani 1 1 d . . . I4 I 0.122122(12) 0.407670(7) 0.637978(7) 0.05611(5) Uani 1 1 d . . . Cu2 Cu 0.43324(3) 0.392972(15) 0.716677(15) 0.06722(11) Uani 1 1 d . . . Cu1 Cu 0.22341(3) 0.352483(15) 0.710350(15) 0.07040(11) Uani 1 1 d . . . Cu4 Cu 0.29552(3) 0.380555(14) 0.611715(13) 0.06321(10) Uani 1 1 d . . . Cu3 Cu 0.26354(3) 0.476062(15) 0.691154(15) 0.07139(11) Uani 1 1 d . . . P1 P 0.13222(5) 0.29513(3) 0.74662(3) 0.0624(2) Uani 1 1 d . . . P3 P 0.21072(5) 0.55911(3) 0.70230(3) 0.05502(19) Uani 1 1 d . . . P4 P 0.30100(5) 0.37499(3) 0.53209(3) 0.05529(19) Uani 1 1 d . . . P2 P 0.59195(5) 0.39117(3) 0.75302(3) 0.0570(2) Uani 1 1 d . . . C33 C 0.63520(19) 0.45127(11) 0.78499(11) 0.0585(8) Uani 1 1 d . . . C14 C 0.30321(19) 0.24529(11) 0.79052(10) 0.0611(8) Uani 1 1 d . . . H14 H 0.3338 0.2768 0.7843 0.073 Uiso 1 1 calc R . . N1 N 0.37490(19) 0.11478(11) 0.84247(12) 0.0845(10) Uani 1 1 d . . . C53 C 0.1719(2) 0.59817(11) 0.64776(11) 0.0611(8) Uani 1 1 d . . . C74 C 0.2470(2) 0.26899(12) 0.52758(11) 0.0670(9) Uani 1 1 d . . . H74 H 0.2285 0.2748 0.5578 0.080 Uiso 1 1 calc R . . C27 C 0.6796(2) 0.38091(12) 0.71114(11) 0.0649(9) Uani 1 1 d . . . C13 C 0.2009(2) 0.24093(10) 0.77750(11) 0.0615(8) Uani 1 1 d . . . C47 C 0.10177(19) 0.56038(11) 0.73275(11) 0.0590(8) Uani 1 1 d . . . C15 C 0.3600(2) 0.20461(12) 0.81225(11) 0.0678(9) Uani 1 1 d . . . H15 H 0.4276 0.2097 0.8206 0.081 Uiso 1 1 calc R . . C41 C 0.2961(2) 0.60203(11) 0.74037(11) 0.0615(8) Uani 1 1 d . . . C73 C 0.2851(2) 0.31050(12) 0.50419(10) 0.0637(8) Uani 1 1 d . . . C61 C 0.2132(2) 0.41883(11) 0.49539(11) 0.0606(8) Uani 1 1 d . . . C67 C 0.4203(2) 0.39671(11) 0.51735(11) 0.0622(8) Uani 1 1 d . . . C78 C 0.3136(3) 0.29807(15) 0.45873(12) 0.0820(11) Uani 1 1 d . . . H78 H 0.3419 0.3243 0.4420 0.098 Uiso 1 1 calc R . . C1 C 0.0344(2) 0.26263(13) 0.70515(13) 0.0782(10) Uani 1 1 d . . . C68 C 0.4297(2) 0.42880(14) 0.47836(13) 0.0823(11) Uani 1 1 d . . . H68 H 0.3740 0.4390 0.4571 0.099 Uiso 1 1 calc R . . C16 C 0.3193(2) 0.15566(11) 0.82226(11) 0.0629(8) Uani 1 1 d . . . C7 C 0.0683(2) 0.32505(13) 0.79267(13) 0.0736(10) Uani 1 1 d . . . C52 C 0.0859(2) 0.59670(15) 0.76694(13) 0.0853(11) Uani 1 1 d . . . H52 H 0.1349 0.6214 0.7771 0.102 Uiso 1 1 calc R . . C21 C 0.6266(2) 0.33893(11) 0.79810(12) 0.0681(9) Uani 1 1 d . . . C22 C 0.7168(2) 0.31415(13) 0.80493(14) 0.0818(12) Uani 1 1 d . . . H22 H 0.7636 0.3227 0.7854 0.098 Uiso 1 1 calc R . . C62 C 0.1927(2) 0.46711(13) 0.51534(13) 0.0770(11) Uani 1 1 d . . . H62 H 0.2241 0.4764 0.5461 0.092 Uiso 1 1 calc R . . C38 C 0.7128(2) 0.45216(13) 0.82408(12) 0.0728(10) Uani 1 1 d . . . H38 H 0.7412 0.4206 0.8363 0.087 Uiso 1 1 calc R . . C75 C 0.2357(3) 0.21890(13) 0.50723(13) 0.0822(11) Uani 1 1 d . . . H75 H 0.2086 0.1923 0.5240 0.099 Uiso 1 1 calc R . . C44 C 0.4245(3) 0.66803(15) 0.80065(16) 0.0973(14) Uani 1 1 d . . . H44 H 0.4657 0.6901 0.8212 0.117 Uiso 1 1 calc R . . N2 N 0.7419(3) 0.59561(11) 0.84962(12) 0.0967(11) Uani 1 1 d . . . C34 C 0.5948(2) 0.50041(13) 0.77027(13) 0.0743(10) Uani 1 1 d . . . H34 H 0.5422 0.5013 0.7450 0.089 Uiso 1 1 calc R . . C18 C 0.1606(2) 0.19278(11) 0.78765(13) 0.0712(10) Uani 1 1 d . . . H18 H 0.0928 0.1881 0.7796 0.085 Uiso 1 1 calc R . . C36 C 0.7062(2) 0.54892(12) 0.82892(11) 0.0666(9) Uani 1 1 d . . . C35 C 0.6283(3) 0.54728(12) 0.79093(13) 0.0801(11) Uani 1 1 d . . . H35 H 0.5983 0.5787 0.7793 0.096 Uiso 1 1 calc R . . C6 C 0.0553(3) 0.24877(13) 0.66033(14) 0.0893(12) Uani 1 1 d . . . H6 H 0.1162 0.2569 0.6514 0.107 Uiso 1 1 calc R . . C43 C 0.3827(2) 0.68494(14) 0.75882(16) 0.0911(13) Uani 1 1 d . . . H43 H 0.3961 0.7190 0.7491 0.109 Uiso 1 1 calc R . . C54 C 0.2249(3) 0.59246(12) 0.60888(13) 0.0836(10) Uani 1 1 d . . . H54 H 0.2763 0.5683 0.6107 0.100 Uiso 1 1 calc R . . C2 C -0.0593(2) 0.25141(14) 0.71828(16) 0.0947(13) Uani 1 1 d . . . H2 H -0.0747 0.2615 0.7482 0.114 Uiso 1 1 calc R . . C77 C 0.3006(3) 0.24822(15) 0.43852(13) 0.0910(12) Uani 1 1 d . . . H77 H 0.3173 0.2423 0.4080 0.109 Uiso 1 1 calc R . . C55 C 0.1998(3) 0.62314(15) 0.56795(14) 0.1068(13) Uani 1 1 d . . . H55 H 0.2367 0.6196 0.5429 0.128 Uiso 1 1 calc R . . C46 C 0.3423(3) 0.58455(15) 0.78429(15) 0.1034(15) Uani 1 1 d . . . H46 H 0.3298 0.5504 0.7940 0.124 Uiso 1 1 calc R . . N4 N 0.2551(3) 0.15734(12) 0.44387(12) 0.1270(15) Uani 1 1 d . . . C37 C 0.7476(2) 0.49996(13) 0.84475(12) 0.0759(10) Uani 1 1 d . . . H37 H 0.8003 0.4995 0.8700 0.091 Uiso 1 1 calc R . . C56 C 0.1239(3) 0.65825(14) 0.56241(12) 0.0806(11) Uani 1 1 d . . . C19 C 0.4808(2) 0.11894(16) 0.84897(18) 0.1121(16) Uani 1 1 d . . . H19A H 0.5017 0.1250 0.8182 0.168 Uiso 1 1 calc R . . H19B H 0.5096 0.0867 0.8628 0.168 Uiso 1 1 calc R . . H19C H 0.5017 0.1479 0.8703 0.168 Uiso 1 1 calc R . . C42 C 0.3183(2) 0.65322(13) 0.72830(14) 0.0812(11) Uani 1 1 d . . . H42 H 0.2890 0.6668 0.6987 0.097 Uiso 1 1 calc R . . C48 C 0.0271(2) 0.52516(13) 0.71735(15) 0.0884(11) Uani 1 1 d . . . H48 H 0.0351 0.5003 0.6938 0.106 Uiso 1 1 calc R . . C17 C 0.2165(2) 0.15141(11) 0.80918(12) 0.0711(9) Uani 1 1 d . . . H17 H 0.1855 0.1200 0.8152 0.085 Uiso 1 1 calc R . . C26 C 0.5562(3) 0.32604(15) 0.82712(14) 0.0892(13) Uani 1 1 d . . . H26 H 0.4950 0.3427 0.8231 0.107 Uiso 1 1 calc R . . C57 C 0.0743(2) 0.66519(14) 0.60250(13) 0.0784(11) Uani 1 1 d . . . H57 H 0.0245 0.6903 0.6010 0.094 Uiso 1 1 calc R . . N3 N 0.1007(3) 0.68936(17) 0.51998(13) 0.1205(14) Uani 1 1 d . . . C58 C 0.0982(2) 0.63548(13) 0.64362(12) 0.0722(9) Uani 1 1 d . . . H58 H 0.0637 0.6407 0.6694 0.087 Uiso 1 1 calc R . . C76 C 0.2634(3) 0.20720(13) 0.46252(13) 0.0848(12) Uani 1 1 d . . . C20 C 0.3334(3) 0.06315(14) 0.84562(15) 0.0921(13) Uani 1 1 d . . . H20A H 0.3066 0.0601 0.8753 0.138 Uiso 1 1 calc R . . H20B H 0.3838 0.0370 0.8450 0.138 Uiso 1 1 calc R . . H20C H 0.2819 0.0577 0.8187 0.138 Uiso 1 1 calc R . . C66 C 0.1643(3) 0.40770(15) 0.45026(15) 0.0963(14) Uani 1 1 d . . . H66 H 0.1757 0.3754 0.4362 0.116 Uiso 1 1 calc R . . C25 C 0.5808(3) 0.28658(16) 0.86313(16) 0.1093(15) Uani 1 1 d . . . H25 H 0.5350 0.2764 0.8827 0.131 Uiso 1 1 calc R . . C63 C 0.1254(3) 0.50159(17) 0.48943(17) 0.1064(15) Uani 1 1 d . . . H63 H 0.1095 0.5328 0.5040 0.128 Uiso 1 1 calc R . . C69 C 0.5232(3) 0.44600(17) 0.47088(15) 0.1031(13) Uani 1 1 d . . . H69 H 0.5286 0.4685 0.4451 0.124 Uiso 1 1 calc R . . C28 C 0.7606(3) 0.41104(16) 0.70853(15) 0.1124(13) Uani 1 1 d . . . H28 H 0.7730 0.4395 0.7297 0.135 Uiso 1 1 calc R . . C12 C 0.0615(3) 0.30505(17) 0.83692(15) 0.1101(15) Uani 1 1 d . . . H12 H 0.0905 0.2725 0.8456 0.132 Uiso 1 1 calc R . . C64 C 0.0828(3) 0.49091(18) 0.44397(17) 0.1083(15) Uani 1 1 d . . . H64 H 0.0435 0.5161 0.4260 0.130 Uiso 1 1 calc R . . C50 C -0.0707(2) 0.56253(15) 0.77206(15) 0.0931(12) Uani 1 1 d . . . H50 H -0.1280 0.5624 0.7861 0.112 Uiso 1 1 calc R . . C32 C 0.6642(3) 0.33878(15) 0.67873(14) 0.0870(12) Uani 1 1 d . . . H32 H 0.6104 0.3166 0.6794 0.104 Uiso 1 1 calc R . . C23 C 0.7373(3) 0.27771(14) 0.83966(16) 0.1016(15) Uani 1 1 d . . . H23 H 0.7988 0.2615 0.8437 0.122 Uiso 1 1 calc R . . C8 C 0.0293(3) 0.37570(16) 0.78416(16) 0.1052(14) Uani 1 1 d . . . H8 H 0.0363 0.3927 0.7554 0.126 Uiso 1 1 calc R . . C51 C 0.0004(3) 0.59814(16) 0.78686(16) 0.0998(13) Uani 1 1 d . . . H51 H -0.0082 0.6233 0.8101 0.120 Uiso 1 1 calc R . . C10 C -0.0283(3) 0.3784(2) 0.85944(17) 0.1184(17) Uani 1 1 d . . . H10 H -0.0628 0.3951 0.8813 0.142 Uiso 1 1 calc R . . C30 C 0.8097(3) 0.36054(18) 0.64593(15) 0.1033(15) Uani 1 1 d . . . H30 H 0.8543 0.3529 0.6250 0.124 Uiso 1 1 calc R . . C45 C 0.4070(3) 0.61581(19) 0.81477(18) 0.1255(18) Uani 1 1 d . . . H45 H 0.4384 0.6026 0.8442 0.151 Uiso 1 1 calc R . . C72 C 0.5046(2) 0.38269(16) 0.54979(15) 0.0928(12) Uani 1 1 d . . . H72 H 0.4992 0.3621 0.5768 0.111 Uiso 1 1 calc R . . C65 C 0.0978(3) 0.44288(18) 0.42451(18) 0.1148(16) Uani 1 1 d . . . H65 H 0.0640 0.4336 0.3943 0.138 Uiso 1 1 calc R . . C70 C 0.6050(2) 0.43073(17) 0.50009(18) 0.1135(15) Uani 1 1 d . . . H70 H 0.6666 0.4405 0.4930 0.136 Uiso 1 1 calc R . . C71 C 0.5985(3) 0.40043(18) 0.54087(19) 0.1148(18) Uani 1 1 d . . . H71 H 0.6552 0.3918 0.5622 0.138 Uiso 1 1 calc R . . C24 C 0.6728(3) 0.26340(15) 0.86898(17) 0.1141(16) Uani 1 1 d . . . H24 H 0.6900 0.2382 0.8929 0.137 Uiso 1 1 calc R . . C9 C -0.0192(3) 0.40135(18) 0.81713(19) 0.1225(17) Uani 1 1 d . . . H9 H -0.0457 0.4348 0.8100 0.147 Uiso 1 1 calc R . . C31 C 0.7261(3) 0.32977(18) 0.64648(15) 0.1057(15) Uani 1 1 d . . . H31 H 0.7125 0.3025 0.6242 0.127 Uiso 1 1 calc R . . C11 C 0.0130(4) 0.3312(2) 0.86962(17) 0.135(2) Uani 1 1 d . . . H11 H 0.0090 0.3156 0.8994 0.161 Uiso 1 1 calc R . . C5 C -0.0173(4) 0.22202(17) 0.62809(17) 0.1267(19) Uani 1 1 d . . . H5 H -0.0039 0.2110 0.5980 0.152 Uiso 1 1 calc R . . C4 C -0.1117(3) 0.21196(19) 0.64190(18) 0.1463(18) Uani 1 1 d . . . H4 H -0.1611 0.1964 0.6199 0.176 Uiso 1 1 calc R . . C49 C -0.0601(3) 0.52649(16) 0.73674(18) 0.1090(15) Uani 1 1 d . . . H49 H -0.1109 0.5031 0.7258 0.131 Uiso 1 1 calc R . . C3 C -0.1288(3) 0.22414(19) 0.68407(19) 0.1280(18) Uani 1 1 d . . . H3 H -0.1892 0.2148 0.6928 0.154 Uiso 1 1 calc R . . C29 C 0.8244(3) 0.4020(2) 0.67679(17) 0.1345(19) Uani 1 1 d . . . H29 H 0.8782 0.4243 0.6763 0.161 Uiso 1 1 calc R . . C39 C 0.8255(4) 0.59454(17) 0.88968(17) 0.1263(18) Uani 1 1 d . . . H39A H 0.8078 0.5742 0.9160 0.189 Uiso 1 1 calc R . . H39B H 0.8414 0.6300 0.9004 0.189 Uiso 1 1 calc R . . H39C H 0.8817 0.5788 0.8787 0.189 Uiso 1 1 calc R . . C79 C 0.2071(5) 0.11704(18) 0.4665(2) 0.192(3) Uani 1 1 d . . . H79A H 0.2555 0.0953 0.4857 0.288 Uiso 1 1 calc R . . H79B H 0.1685 0.0957 0.4422 0.288 Uiso 1 1 calc R . . H79C H 0.1648 0.1327 0.4869 0.288 Uiso 1 1 calc R . . C59 C 0.1398(6) 0.6728(3) 0.4766(2) 0.304(4) Uani 1 1 d . . . H59A H 0.1357 0.6350 0.4736 0.455 Uiso 1 1 calc R . . H59B H 0.2075 0.6836 0.4790 0.455 Uiso 1 1 calc R . . H59C H 0.1020 0.6889 0.4486 0.455 Uiso 1 1 calc R . . C60 C 0.0052(4) 0.7113(3) 0.5100(2) 0.222(3) Uani 1 1 d . . . H60A H -0.0421 0.6860 0.5179 0.333 Uiso 1 1 calc R . . H60B H -0.0094 0.7202 0.4763 0.333 Uiso 1 1 calc R . . H60C H 0.0022 0.7426 0.5292 0.333 Uiso 1 1 calc R . . C40 C 0.7085(4) 0.64505(14) 0.8291(2) 0.124(2) Uani 1 1 d . . . H40A H 0.7306 0.6493 0.7984 0.185 Uiso 1 1 calc R . . H40B H 0.7346 0.6731 0.8504 0.185 Uiso 1 1 calc R . . H40C H 0.6378 0.6461 0.8247 0.185 Uiso 1 1 calc R . . C80 C 0.2919(4) 0.14408(18) 0.39896(16) 0.140(2) Uani 1 1 d . . . H80A H 0.2834 0.1739 0.3775 0.210 Uiso 1 1 calc R . . H80B H 0.2558 0.1144 0.3839 0.210 Uiso 1 1 calc R . . H80C H 0.3606 0.1352 0.4061 0.210 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.06040(9) 0.04476(8) 0.06488(10) 0.00336(7) 0.00860(7) 0.00150(7) I3 0.05577(8) 0.05104(8) 0.06139(9) 0.00456(7) 0.01300(7) -0.00557(7) I2 0.07154(10) 0.05583(9) 0.05798(10) 0.00550(7) 0.01493(8) 0.00158(8) I4 0.05064(8) 0.05799(9) 0.06049(9) 0.00783(7) 0.01108(7) 0.00576(7) Cu2 0.05804(18) 0.0665(2) 0.0757(2) 0.00150(18) 0.00579(16) -0.00158(16) Cu1 0.0733(2) 0.06082(19) 0.0783(2) 0.01666(17) 0.01561(17) -0.00164(17) Cu4 0.07014(18) 0.06350(18) 0.05812(18) 0.00373(15) 0.01661(15) 0.00233(16) Cu3 0.0803(2) 0.06127(19) 0.0763(2) 0.00688(17) 0.02391(17) 0.01454(17) P1 0.0579(4) 0.0579(4) 0.0711(4) 0.0157(3) 0.0087(3) 0.0007(3) P3 0.0565(3) 0.0495(3) 0.0600(4) 0.0031(3) 0.0123(3) 0.0029(3) P4 0.0606(3) 0.0548(3) 0.0514(3) 0.0041(3) 0.0117(3) -0.0004(3) P2 0.0548(3) 0.0485(3) 0.0669(4) -0.0020(3) 0.0064(3) -0.0008(3) C33 0.0575(14) 0.0512(13) 0.0669(16) -0.0048(12) 0.0105(12) -0.0003(11) C14 0.0610(14) 0.0573(14) 0.0639(16) 0.0139(12) 0.0061(12) -0.0099(12) N1 0.0764(16) 0.0657(14) 0.110(2) 0.0297(14) 0.0104(15) 0.0135(13) C53 0.0674(15) 0.0559(14) 0.0608(15) -0.0011(12) 0.0128(12) 0.0044(12) C74 0.0807(17) 0.0634(16) 0.0590(16) -0.0039(13) 0.0177(13) -0.0085(14) C27 0.0502(13) 0.0667(16) 0.0752(18) -0.0102(14) 0.0010(13) 0.0011(13) C13 0.0604(14) 0.0482(12) 0.0745(17) 0.0127(12) 0.0058(13) -0.0045(12) C47 0.0567(13) 0.0537(13) 0.0684(16) 0.0050(12) 0.0152(11) -0.0011(11) C15 0.0582(14) 0.0729(17) 0.0716(17) 0.0190(14) 0.0078(13) -0.0012(13) C41 0.0631(14) 0.0607(15) 0.0624(16) -0.0032(12) 0.0147(12) 0.0018(12) C73 0.0676(15) 0.0699(16) 0.0550(15) 0.0077(13) 0.0138(12) 0.0004(13) C61 0.0545(13) 0.0641(15) 0.0623(16) 0.0149(12) 0.0057(12) -0.0021(12) C67 0.0587(13) 0.0614(15) 0.0694(16) 0.0039(13) 0.0186(12) -0.0019(12) C78 0.107(2) 0.086(2) 0.0568(17) -0.0016(15) 0.0252(15) -0.0059(18) C1 0.0690(17) 0.0680(16) 0.090(2) 0.0313(15) -0.0120(16) -0.0043(14) C68 0.0852(18) 0.091(2) 0.0716(19) 0.0174(16) 0.0129(15) -0.0261(16) C16 0.0661(15) 0.0576(14) 0.0667(16) 0.0069(12) 0.0154(12) 0.0033(12) C7 0.0636(16) 0.0758(18) 0.083(2) 0.0195(15) 0.0149(14) 0.0086(14) C52 0.0832(18) 0.091(2) 0.089(2) -0.0239(17) 0.0379(15) -0.0090(16) C21 0.0735(17) 0.0524(14) 0.0745(19) 0.0006(14) -0.0014(15) -0.0032(13) C22 0.0739(18) 0.0684(18) 0.096(2) 0.0081(18) -0.0094(18) 0.0097(16) C62 0.0701(17) 0.0789(19) 0.084(2) 0.0110(16) 0.0189(15) 0.0090(15) C38 0.0769(18) 0.0617(16) 0.077(2) 0.0024(15) 0.0046(16) 0.0005(15) C75 0.110(2) 0.0565(16) 0.082(2) -0.0017(15) 0.0217(18) -0.0118(16) C44 0.097(2) 0.072(2) 0.110(3) -0.003(2) -0.027(2) -0.0111(19) N2 0.122(2) 0.0705(15) 0.099(2) -0.0339(14) 0.0213(18) -0.0222(16) C34 0.0723(18) 0.0623(16) 0.083(2) -0.0027(16) -0.0058(16) -0.0035(15) C18 0.0585(15) 0.0577(15) 0.095(2) 0.0174(15) 0.0048(15) 0.0005(13) C36 0.0709(16) 0.0621(15) 0.0684(17) -0.0064(13) 0.0165(13) -0.0052(13) C35 0.113(2) 0.0425(13) 0.084(2) -0.0018(14) 0.0111(19) 0.0039(16) C6 0.109(2) 0.0647(18) 0.085(2) 0.0146(17) -0.015(2) -0.0074(18) C43 0.0764(19) 0.0702(19) 0.123(3) -0.001(2) 0.003(2) -0.0198(16) C54 0.109(2) 0.0690(16) 0.079(2) 0.0128(15) 0.0344(16) 0.0377(15) C2 0.0661(18) 0.079(2) 0.132(3) 0.031(2) -0.009(2) -0.0052(17) C77 0.144(3) 0.079(2) 0.0546(17) -0.0018(15) 0.0283(18) -0.004(2) C55 0.156(3) 0.092(2) 0.084(2) 0.0347(17) 0.0565(19) 0.048(2) C46 0.130(3) 0.073(2) 0.093(3) -0.0026(19) -0.028(2) -0.008(2) N4 0.244(4) 0.0710(17) 0.0739(18) -0.0274(14) 0.050(2) -0.031(2) C37 0.0780(19) 0.0800(19) 0.0643(18) -0.0145(15) -0.0066(15) -0.0027(16) C56 0.098(2) 0.085(2) 0.0602(18) 0.0092(16) 0.0166(16) 0.0072(18) C19 0.069(2) 0.106(3) 0.160(4) 0.048(3) 0.015(2) 0.017(2) C42 0.0788(19) 0.0690(18) 0.092(2) 0.0066(17) -0.0002(18) -0.0104(16) C48 0.0856(18) 0.0662(17) 0.123(2) -0.0243(17) 0.0470(16) -0.0102(15) C17 0.0736(17) 0.0542(14) 0.084(2) 0.0173(13) 0.0089(15) -0.0104(13) C26 0.083(2) 0.094(2) 0.086(2) 0.0270(19) -0.0010(18) 0.0046(19) C57 0.0601(16) 0.093(2) 0.078(2) 0.0181(17) -0.0003(15) 0.0142(16) N3 0.134(3) 0.147(3) 0.078(2) 0.0425(19) 0.0078(19) 0.035(2) C58 0.0727(16) 0.0824(19) 0.0634(17) 0.0137(14) 0.0166(13) 0.0241(14) C76 0.119(3) 0.0679(18) 0.0680(19) -0.0182(15) 0.0160(18) -0.0125(18) C20 0.088(2) 0.077(2) 0.110(3) 0.018(2) 0.011(2) 0.0220(18) C66 0.110(3) 0.078(2) 0.089(3) 0.005(2) -0.022(2) 0.001(2) C25 0.130(3) 0.095(2) 0.100(3) 0.027(2) 0.005(2) -0.029(2) C63 0.099(2) 0.089(2) 0.130(3) 0.028(2) 0.016(2) 0.034(2) C69 0.115(2) 0.103(3) 0.104(2) 0.015(2) 0.0558(17) -0.013(2) C28 0.114(2) 0.111(2) 0.128(3) -0.0561(19) 0.0675(18) -0.0514(18) C12 0.148(3) 0.103(3) 0.089(2) 0.030(2) 0.045(2) 0.043(2) C64 0.084(2) 0.111(3) 0.120(3) 0.039(2) -0.016(2) 0.009(2) C50 0.0792(17) 0.089(2) 0.121(3) 0.006(2) 0.0477(16) 0.0097(17) C32 0.0743(19) 0.088(2) 0.100(3) -0.0175(19) 0.0157(18) 0.0008(17) C23 0.103(3) 0.072(2) 0.123(3) 0.013(2) -0.006(2) 0.0217(19) C8 0.088(2) 0.112(3) 0.124(3) 0.043(2) 0.0424(18) 0.0362(19) C51 0.0840(19) 0.099(2) 0.125(3) -0.030(2) 0.0443(18) 0.0025(18) C10 0.113(3) 0.144(4) 0.107(3) 0.001(3) 0.043(2) 0.026(3) C30 0.091(2) 0.131(3) 0.090(2) -0.024(2) 0.0213(19) 0.015(2) C45 0.134(3) 0.113(3) 0.109(3) 0.002(3) -0.047(3) -0.022(3) C72 0.0703(17) 0.104(2) 0.108(2) 0.035(2) 0.0272(17) 0.0203(18) C65 0.092(2) 0.114(3) 0.122(3) 0.025(3) -0.037(2) 0.004(2) C70 0.0728(17) 0.102(3) 0.180(4) 0.004(3) 0.0632(19) 0.0076(19) C71 0.0580(18) 0.120(3) 0.168(4) 0.029(3) 0.025(2) 0.018(2) C24 0.141(3) 0.0588(19) 0.124(3) 0.014(2) -0.038(3) 0.007(2) C9 0.129(3) 0.108(3) 0.140(4) 0.032(3) 0.048(3) 0.055(2) C31 0.112(3) 0.116(3) 0.090(3) -0.033(2) 0.016(2) 0.013(2) C11 0.166(3) 0.164(4) 0.086(3) 0.010(3) 0.060(2) 0.025(3) C5 0.186(4) 0.086(3) 0.089(3) 0.013(2) -0.036(3) 0.023(3) C4 0.150(3) 0.112(3) 0.142(3) 0.037(3) -0.087(2) -0.044(3) C49 0.0840(19) 0.087(2) 0.168(4) -0.015(2) 0.055(2) -0.0270(17) C3 0.088(2) 0.121(3) 0.156(4) 0.045(3) -0.043(2) -0.017(2) C29 0.099(2) 0.191(5) 0.127(3) -0.057(3) 0.060(2) -0.048(3) C39 0.159(4) 0.095(3) 0.114(3) -0.041(2) -0.015(3) -0.033(3) C79 0.371(8) 0.069(2) 0.150(5) -0.033(3) 0.083(5) -0.048(4) C59 0.562(9) 0.276(6) 0.110(3) 0.111(3) 0.172(4) 0.261(5) C60 0.112(4) 0.351(7) 0.196(4) 0.180(4) 0.003(3) 0.040(4) C40 0.152(4) 0.059(2) 0.159(4) -0.012(2) 0.022(3) -0.005(2) C80 0.223(5) 0.111(3) 0.092(3) -0.039(2) 0.041(3) 0.005(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 I1 Cu4 2.6701(6) . ? I1 Cu2 2.7144(6) . ? I1 Cu1 2.7382(6) . ? I3 Cu3 2.6315(7) . ? I3 Cu2 2.7184(7) . ? I3 Cu4 2.7632(6) . ? I2 Cu2 2.6763(6) . ? I2 Cu1 2.6978(6) . ? I2 Cu3 2.7118(7) . ? I4 Cu1 2.6677(6) . ? I4 Cu4 2.6846(7) . ? I4 Cu3 2.8440(6) . ? Cu2 P2 2.2582(9) . ? Cu2 Cu1 3.0357(8) . ? Cu1 P1 2.2559(10) . ? Cu4 P4 2.2439(10) . ? Cu3 P3 2.2600(9) . ? P1 C13 1.807(3) . ? P1 C1 1.829(3) . ? P1 C7 1.829(4) . ? P3 C41 1.818(3) . ? P3 C53 1.827(3) . ? P3 C47 1.831(3) . ? P4 C73 1.808(3) . ? P4 C61 1.832(3) . ? P4 C67 1.833(3) . ? P2 C33 1.817(3) . ? P2 C27 1.822(3) . ? P2 C21 1.838(3) . ? C33 C34 1.397(4) . ? C33 C38 1.405(4) . ? C14 C15 1.375(4) . ? C14 C13 1.399(4) . ? N1 C16 1.357(4) . ? N1 C20 1.433(4) . ? N1 C19 1.440(4) . ? C53 C58 1.376(4) . ? C53 C54 1.404(5) . ? C74 C73 1.382(4) . ? C74 C75 1.388(4) . ? C27 C28 1.358(5) . ? C27 C32 1.394(5) . ? C13 C18 1.385(4) . ? C47 C52 1.368(5) . ? C47 C48 1.376(4) . ? C15 C16 1.405(4) . ? C41 C46 1.367(5) . ? C41 C42 1.384(4) . ? C73 C78 1.421(5) . ? C61 C66 1.365(5) . ? C61 C62 1.390(4) . ? C67 C68 1.382(5) . ? C67 C72 1.402(4) . ? C78 C77 1.383(5) . ? C1 C6 1.374(5) . ? C1 C2 1.419(5) . ? C68 C69 1.399(5) . ? C16 C17 1.405(4) . ? C7 C12 1.354(5) . ? C7 C8 1.395(5) . ? C52 C51 1.374(5) . ? C21 C22 1.375(4) . ? C21 C26 1.392(5) . ? C22 C23 1.337(5) . ? C62 C63 1.391(5) . ? C38 C37 1.393(5) . ? C75 C76 1.393(5) . ? C44 C43 1.294(6) . ? C44 C45 1.410(6) . ? N2 C36 1.373(4) . ? N2 C40 1.422(5) . ? N2 C39 1.476(5) . ? C34 C35 1.367(4) . ? C18 C17 1.381(4) . ? C36 C35 1.388(4) . ? C36 C37 1.406(4) . ? C6 C5 1.410(6) . ? C43 C42 1.387(5) . ? C54 C55 1.382(5) . ? C2 C3 1.422(6) . ? C77 C76 1.376(5) . ? C55 C56 1.359(5) . ? C46 C45 1.381(6) . ? N4 C76 1.363(5) . ? N4 C79 1.414(7) . ? N4 C80 1.463(6) . ? C56 C57 1.409(5) . ? C56 N3 1.419(5) . ? C48 C49 1.388(5) . ? C26 C25 1.422(6) . ? C57 C58 1.371(5) . ? N3 C60 1.410(6) . ? N3 C59 1.461(8) . ? C66 C65 1.393(6) . ? C25 C24 1.379(6) . ? C63 C64 1.343(6) . ? C69 C70 1.341(5) . ? C28 C29 1.359(6) . ? C12 C11 1.381(7) . ? C64 C65 1.360(7) . ? C50 C51 1.346(5) . ? C50 C49 1.368(6) . ? C32 C31 1.350(6) . ? C23 C24 1.345(7) . ? C8 C9 1.379(7) . ? C10 C11 1.332(7) . ? C10 C9 1.341(7) . ? C30 C29 1.353(7) . ? C30 C31 1.389(6) . ? C72 C71 1.423(5) . ? C70 C71 1.388(7) . ? C5 C4 1.430(7) . ? C4 C3 1.275(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu4 I1 Cu2 74.35(2) . . ? Cu4 I1 Cu1 71.258(18) . . ? Cu2 I1 Cu1 67.660(18) . . ? Cu3 I3 Cu2 71.790(17) . . ? Cu3 I3 Cu4 76.914(18) . . ? Cu2 I3 Cu4 72.819(19) . . ? Cu2 I2 Cu1 68.787(19) . . ? Cu2 I2 Cu3 71.222(19) . . ? Cu1 I2 Cu3 73.44(2) . . ? Cu1 I4 Cu4 72.132(18) . . ? Cu1 I4 Cu3 71.78(2) . . ? Cu4 I4 Cu3 74.706(19) . . ? P2 Cu2 I2 113.11(3) . . ? P2 Cu2 I1 114.80(2) . . ? I2 Cu2 I1 110.031(18) . . ? P2 Cu2 I3 108.96(3) . . ? I2 Cu2 I3 105.89(2) . . ? I1 Cu2 I3 103.19(2) . . ? P2 Cu2 Cu1 149.33(3) . . ? I2 Cu2 Cu1 55.941(16) . . ? I1 Cu2 Cu1 56.544(12) . . ? I3 Cu2 Cu1 101.709(15) . . ? P1 Cu1 I4 114.67(3) . . ? P1 Cu1 I2 109.36(3) . . ? I4 Cu1 I2 106.83(2) . . ? P1 Cu1 I1 111.86(3) . . ? I4 Cu1 I1 105.15(2) . . ? I2 Cu1 I1 108.68(2) . . ? P1 Cu1 Cu2 141.02(3) . . ? I4 Cu1 Cu2 104.292(19) . . ? I2 Cu1 Cu2 55.272(13) . . ? I1 Cu1 Cu2 55.796(17) . . ? P4 Cu4 I1 119.90(3) . . ? P4 Cu4 I4 116.96(2) . . ? I1 Cu4 I4 106.599(17) . . ? P4 Cu4 I3 105.42(2) . . ? I1 Cu4 I3 103.16(2) . . ? I4 Cu4 I3 102.424(19) . . ? P3 Cu3 I3 117.24(3) . . ? P3 Cu3 I2 111.82(3) . . ? I3 Cu3 I2 107.356(19) . . ? P3 Cu3 I4 115.49(3) . . ? I3 Cu3 I4 101.65(2) . . ? I2 Cu3 I4 101.67(2) . . ? C13 P1 C1 103.89(14) . . ? C13 P1 C7 104.41(15) . . ? C1 P1 C7 104.37(15) . . ? C13 P1 Cu1 114.74(10) . . ? C1 P1 Cu1 114.07(12) . . ? C7 P1 Cu1 114.14(11) . . ? C41 P3 C53 104.18(13) . . ? C41 P3 C47 102.50(14) . . ? C53 P3 C47 102.98(13) . . ? C41 P3 Cu3 116.41(10) . . ? C53 P3 Cu3 116.51(10) . . ? C47 P3 Cu3 112.49(9) . . ? C73 P4 C61 106.21(13) . . ? C73 P4 C67 103.09(14) . . ? C61 P4 C67 103.04(13) . . ? C73 P4 Cu4 117.70(10) . . ? C61 P4 Cu4 113.51(10) . . ? C67 P4 Cu4 111.79(10) . . ? C33 P2 C27 103.74(14) . . ? C33 P2 C21 103.52(14) . . ? C27 P2 C21 102.22(15) . . ? C33 P2 Cu2 115.11(9) . . ? C27 P2 Cu2 113.58(10) . . ? C21 P2 Cu2 116.96(10) . . ? C34 C33 C38 115.7(3) . . ? C34 C33 P2 121.0(2) . . ? C38 C33 P2 123.2(2) . . ? C15 C14 C13 122.3(3) . . ? C16 N1 C20 121.1(3) . . ? C16 N1 C19 119.3(3) . . ? C20 N1 C19 117.5(3) . . ? C58 C53 C54 117.8(3) . . ? C58 C53 P3 123.9(2) . . ? C54 C53 P3 118.2(2) . . ? C73 C74 C75 121.8(3) . . ? C28 C27 C32 116.0(3) . . ? C28 C27 P2 125.5(3) . . ? C32 C27 P2 118.5(2) . . ? C18 C13 C14 115.6(2) . . ? C18 C13 P1 124.7(2) . . ? C14 C13 P1 119.6(2) . . ? C52 C47 C48 117.6(3) . . ? C52 C47 P3 124.5(2) . . ? C48 C47 P3 117.7(2) . . ? C14 C15 C16 122.1(3) . . ? C46 C41 C42 115.7(3) . . ? C46 C41 P3 120.1(3) . . ? C42 C41 P3 124.2(2) . . ? C74 C73 C78 115.5(3) . . ? C74 C73 P4 120.8(2) . . ? C78 C73 P4 123.7(2) . . ? C66 C61 C62 116.8(3) . . ? C66 C61 P4 125.5(3) . . ? C62 C61 P4 117.6(2) . . ? C68 C67 C72 119.4(3) . . ? C68 C67 P4 123.3(2) . . ? C72 C67 P4 117.1(2) . . ? C77 C78 C73 122.1(3) . . ? C6 C1 C2 120.6(3) . . ? C6 C1 P1 117.2(3) . . ? C2 C1 P1 122.1(3) . . ? C67 C68 C69 120.0(3) . . ? N1 C16 C17 121.9(3) . . ? N1 C16 C15 122.6(3) . . ? C17 C16 C15 115.5(3) . . ? C12 C7 C8 114.9(4) . . ? C12 C7 P1 126.6(3) . . ? C8 C7 P1 118.2(3) . . ? C47 C52 C51 122.6(3) . . ? C22 C21 C26 120.2(3) . . ? C22 C21 P2 123.8(3) . . ? C26 C21 P2 116.0(2) . . ? C23 C22 C21 120.0(4) . . ? C61 C62 C63 120.1(3) . . ? C37 C38 C33 120.5(3) . . ? C74 C75 C76 122.2(3) . . ? C43 C44 C45 119.5(4) . . ? C36 N2 C40 121.0(3) . . ? C36 N2 C39 119.3(3) . . ? C40 N2 C39 119.1(3) . . ? C35 C34 C33 123.7(3) . . ? C17 C18 C13 122.9(3) . . ? N2 C36 C35 122.1(3) . . ? N2 C36 C37 121.7(3) . . ? C35 C36 C37 116.2(3) . . ? C34 C35 C36 121.3(3) . . ? C1 C6 C5 118.7(4) . . ? C44 C43 C42 121.2(4) . . ? C55 C54 C53 119.4(3) . . ? C1 C2 C3 117.7(4) . . ? C76 C77 C78 121.5(3) . . ? C56 C55 C54 123.4(4) . . ? C41 C46 C45 122.3(4) . . ? C76 N4 C79 120.9(4) . . ? C76 N4 C80 121.4(4) . . ? C79 N4 C80 117.7(4) . . ? C38 C37 C36 122.6(3) . . ? C55 C56 C57 116.5(3) . . ? C55 C56 N3 121.9(4) . . ? C57 C56 N3 121.5(3) . . ? C41 C42 C43 122.3(3) . . ? C47 C48 C49 120.5(3) . . ? C18 C17 C16 121.6(3) . . ? C21 C26 C25 117.8(3) . . ? C58 C57 C56 121.1(3) . . ? C60 N3 C56 117.8(4) . . ? C60 N3 C59 113.4(4) . . ? C56 N3 C59 118.1(4) . . ? C57 C58 C53 121.7(3) . . ? N4 C76 C77 121.8(4) . . ? N4 C76 C75 121.4(3) . . ? C77 C76 C75 116.7(3) . . ? C61 C66 C65 122.4(4) . . ? C24 C25 C26 119.8(4) . . ? C64 C63 C62 121.7(4) . . ? C70 C69 C68 121.4(4) . . ? C27 C28 C29 123.7(4) . . ? C7 C12 C11 122.3(4) . . ? C63 C64 C65 119.2(4) . . ? C51 C50 C49 121.1(4) . . ? C31 C32 C27 121.0(3) . . ? C22 C23 C24 122.9(4) . . ? C9 C8 C7 122.0(4) . . ? C50 C51 C52 118.8(4) . . ? C11 C10 C9 118.9(5) . . ? C29 C30 C31 118.0(4) . . ? C46 C45 C44 119.0(4) . . ? C67 C72 C71 119.1(4) . . ? C64 C65 C66 119.4(4) . . ? C69 C70 C71 120.4(4) . . ? C70 C71 C72 119.5(4) . . ? C23 C24 C25 119.3(4) . . ? C10 C9 C8 120.4(4) . . ? C32 C31 C30 121.2(4) . . ? C10 C11 C12 121.4(5) . . ? C6 C5 C4 119.6(4) . . ? C3 C4 C5 120.6(4) . . ? C50 C49 C48 119.4(3) . . ? C4 C3 C2 122.7(4) . . ? C30 C29 C28 119.9(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.700 _refine_diff_density_min -1.441 _refine_diff_density_rms 0.191 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.089 0.500 0.000 1074.6 4.6 2 0.076 1.000 0.500 1074.7 4.1 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 928675' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global ################################################################### data_1d #TrackingRef '1c&1d.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 4(C20H20NPCuI) _chemical_formula_sum 'C80 H80 Cu4 I4 N4 P4' _chemical_formula_weight 1983.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.663(2) _cell_length_b 25.134(4) _cell_length_c 28.011(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.145(3) _cell_angle_gamma 90.00 _cell_volume 9522(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25508 _cell_measurement_theta_min 2.3892 _cell_measurement_theta_max 27.5204 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 2.282 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3413 _exptl_absorpt_correction_T_max 0.5476 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74734 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.49 _reflns_number_total 21675 _reflns_number_gt 14695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0954P)^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 21675 _refine_ls_number_parameters 870 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1686 _refine_ls_wR_factor_gt 0.1523 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.13213(3) 0.306116(13) 0.327282(13) 0.05170(10) Uani 1 1 d . . . I2 I 0.19041(3) 0.429209(15) 0.223807(13) 0.05778(11) Uani 1 1 d . . . I3 I 0.08646(2) 0.468469(13) 0.357086(12) 0.05119(10) Uani 1 1 d . . . I4 I 0.37685(2) 0.412367(14) 0.360099(12) 0.05185(10) Uani 1 1 d . . . Cu2 Cu 0.06638(5) 0.39760(3) 0.28377(3) 0.06184(18) Uani 1 1 d . . . Cu4 Cu 0.20601(5) 0.38187(3) 0.38776(2) 0.06011(18) Uani 1 1 d . . . Cu3 Cu 0.23565(6) 0.48073(3) 0.30830(3) 0.0661(2) Uani 1 1 d . . . P4 P 0.20168(10) 0.37471(6) 0.46707(5) 0.0508(3) Uani 1 1 d . . . P2 P -0.09238(10) 0.39701(6) 0.24855(5) 0.0515(3) Uani 1 1 d . . . P1 P 0.37025(11) 0.30178(6) 0.25017(6) 0.0591(4) Uani 1 1 d . . . P3 P 0.28919(10) 0.56389(6) 0.29778(5) 0.0502(3) Uani 1 1 d . . . Cu1 Cu 0.27761(6) 0.35794(3) 0.28756(3) 0.0677(2) Uani 1 1 d . . . C53 C 0.3270(4) 0.6036(2) 0.35176(19) 0.0521(12) Uani 1 1 d . . . C33 C -0.1342(4) 0.4569(2) 0.21658(19) 0.0520(12) Uani 1 1 d . . . C15 C 0.1455(4) 0.2090(2) 0.1863(2) 0.0632(14) Uani 1 1 d . . . H15 H 0.0775 0.2132 0.1784 0.076 Uiso 1 1 calc R . . C27 C -0.1825(4) 0.3879(2) 0.2904(2) 0.0579(13) Uani 1 1 d . . . C73 C 0.2159(4) 0.3090(2) 0.49546(19) 0.0555(13) Uani 1 1 d . . . C13 C 0.3034(4) 0.2475(2) 0.2191(2) 0.0588(13) Uani 1 1 d . . . C47 C 0.3994(4) 0.5655(2) 0.2677(2) 0.0528(12) Uani 1 1 d . . . C1 C 0.4707(5) 0.2695(3) 0.2895(3) 0.0709(17) Uani 1 1 d . . . C14 C 0.2008(4) 0.2507(3) 0.2077(2) 0.0613(14) Uani 1 1 d . . . H14 H 0.1688 0.2818 0.2146 0.074 Uiso 1 1 calc R . . C41 C 0.2039(4) 0.6089(2) 0.2606(2) 0.0550(12) Uani 1 1 d . . . N1 N 0.1304(4) 0.1201(2) 0.1548(2) 0.0818(16) Uani 1 1 d . . . C74 C 0.1924(5) 0.2983(3) 0.5406(2) 0.0711(17) Uani 1 1 d . . . H74 H 0.1684 0.3261 0.5575 0.085 Uiso 1 1 calc R . . C16 C 0.1881(5) 0.1607(2) 0.1761(2) 0.0643(15) Uani 1 1 d . . . C78 C 0.2529(5) 0.2675(2) 0.4709(2) 0.0631(14) Uani 1 1 d . . . H78 H 0.2697 0.2733 0.4403 0.076 Uiso 1 1 calc R . . C58 C 0.3969(5) 0.6422(2) 0.3549(2) 0.0636(15) Uani 1 1 d . . . H58 H 0.4290 0.6486 0.3283 0.076 Uiso 1 1 calc R . . C67 C 0.0830(4) 0.3972(2) 0.4828(2) 0.0582(13) Uani 1 1 d . . . C7 C 0.4317(4) 0.3334(2) 0.2045(2) 0.0668(15) Uani 1 1 d . . . C77 C 0.2650(5) 0.2175(2) 0.4913(2) 0.0697(16) Uani 1 1 d . . . H77 H 0.2895 0.1904 0.4738 0.084 Uiso 1 1 calc R . . C22 C -0.2200(5) 0.3212(3) 0.1963(3) 0.0725(17) Uani 1 1 d . . . H22 H -0.2660 0.3302 0.2165 0.087 Uiso 1 1 calc R . . C61 C 0.2917(4) 0.4170(2) 0.5033(2) 0.0632(15) Uani 1 1 d . . . C48 C 0.4763(5) 0.5318(3) 0.2846(3) 0.084(2) Uani 1 1 d . . . H48 H 0.4697 0.5076 0.3091 0.101 Uiso 1 1 calc R . . C18 C 0.3460(4) 0.1989(2) 0.2086(2) 0.0654(15) Uani 1 1 d . . . H18 H 0.4141 0.1944 0.2157 0.078 Uiso 1 1 calc R . . C21 C -0.1263(4) 0.3453(2) 0.2034(2) 0.0594(13) Uani 1 1 d . . . C75 C 0.2019(5) 0.2502(3) 0.5620(2) 0.0758(17) Uani 1 1 d . . . H75 H 0.1833 0.2451 0.5923 0.091 Uiso 1 1 calc R . . C57 C 0.4224(5) 0.6724(3) 0.3964(3) 0.0762(18) Uani 1 1 d . . . H57 H 0.4696 0.6991 0.3968 0.091 Uiso 1 1 calc R . . C68 C 0.0745(6) 0.4312(3) 0.5224(3) 0.085(2) Uani 1 1 d . . . H68 H 0.1295 0.4452 0.5416 0.102 Uiso 1 1 calc R . . C38 C -0.2089(5) 0.4594(2) 0.1782(2) 0.0688(16) Uani 1 1 d . . . H38 H -0.2389 0.4279 0.1665 0.083 Uiso 1 1 calc R . . C76 C 0.2420(5) 0.2062(3) 0.5365(2) 0.0729(17) Uani 1 1 d . . . C46 C 0.1666(7) 0.5933(3) 0.2152(3) 0.094(2) Uani 1 1 d . . . H46 H 0.1832 0.5602 0.2040 0.113 Uiso 1 1 calc R . . C36 C -0.1978(5) 0.5553(3) 0.1733(2) 0.0678(16) Uani 1 1 d . . . C34 C -0.0916(5) 0.5065(3) 0.2327(3) 0.0761(18) Uani 1 1 d . . . H34 H -0.0405 0.5074 0.2584 0.091 Uiso 1 1 calc R . . C20 C 0.1705(6) 0.0683(3) 0.1530(3) 0.095(2) Uani 1 1 d . . . H20A H 0.2215 0.0685 0.1326 0.143 Uiso 1 1 calc R . . H20B H 0.1192 0.0440 0.1401 0.143 Uiso 1 1 calc R . . H20C H 0.1980 0.0573 0.1849 0.143 Uiso 1 1 calc R . . C32 C -0.1638(5) 0.3490(3) 0.3241(3) 0.085(2) Uani 1 1 d . . . H32 H -0.1063 0.3289 0.3257 0.102 Uiso 1 1 calc R . . C56 C 0.3782(5) 0.6632(3) 0.4371(2) 0.0749(18) Uani 1 1 d . . . C12 C 0.4454(6) 0.3098(3) 0.1607(3) 0.085(2) Uani 1 1 d . . . H12 H 0.4218 0.2758 0.1530 0.102 Uiso 1 1 calc R . . C43 C 0.1135(5) 0.6915(3) 0.2467(3) 0.082(2) Uani 1 1 d . . . H43 H 0.0972 0.7248 0.2576 0.099 Uiso 1 1 calc R . . C55 C 0.3091(7) 0.6242(3) 0.4338(3) 0.108(3) Uani 1 1 d . . . H55 H 0.2779 0.6174 0.4606 0.129 Uiso 1 1 calc R . . C26 C -0.0561(5) 0.3321(3) 0.1744(3) 0.0758(18) Uani 1 1 d . . . H26 H 0.0057 0.3484 0.1776 0.091 Uiso 1 1 calc R . . C23 C -0.2446(6) 0.2855(3) 0.1611(3) 0.086(2) Uani 1 1 d . . . H23 H -0.3079 0.2711 0.1560 0.103 Uiso 1 1 calc R . . C35 C -0.1252(5) 0.5524(2) 0.2109(3) 0.0793(19) Uani 1 1 d . . . H35 H -0.0961 0.5840 0.2228 0.095 Uiso 1 1 calc R . . C62 C 0.3440(6) 0.4024(3) 0.5464(3) 0.089(2) Uani 1 1 d . . . H62 H 0.3371 0.3683 0.5585 0.106 Uiso 1 1 calc R . . C52 C 0.4108(6) 0.5988(4) 0.2314(3) 0.099(3) Uani 1 1 d . . . H52 H 0.3583 0.6205 0.2189 0.119 Uiso 1 1 calc R . . C8 C 0.4693(6) 0.3854(3) 0.2123(3) 0.089(2) Uani 1 1 d . . . H8 H 0.4621 0.4024 0.2411 0.107 Uiso 1 1 calc R . . C37 C -0.2417(5) 0.5073(3) 0.1562(2) 0.0816(19) Uani 1 1 d . . . H37 H -0.2924 0.5073 0.1302 0.098 Uiso 1 1 calc R . . C6 C 0.4514(6) 0.2543(3) 0.3351(3) 0.086(2) Uani 1 1 d . . . H6 H 0.3899 0.2612 0.3443 0.104 Uiso 1 1 calc R . . C2 C 0.5616(5) 0.2578(3) 0.2757(3) 0.092(2) Uani 1 1 d . . . H2 H 0.5753 0.2677 0.2454 0.110 Uiso 1 1 calc R . . C30 C -0.3156(6) 0.3701(4) 0.3548(3) 0.109(3) Uani 1 1 d . . . H30 H -0.3591 0.3648 0.3770 0.130 Uiso 1 1 calc R . . C24 C -0.1736(7) 0.2699(3) 0.1319(3) 0.097(3) Uani 1 1 d . . . H24 H -0.1887 0.2446 0.1078 0.116 Uiso 1 1 calc R . . C54 C 0.2823(6) 0.5937(3) 0.3925(3) 0.088(2) Uani 1 1 d . . . H54 H 0.2351 0.5669 0.3922 0.105 Uiso 1 1 calc R . . C19 C 0.0272(6) 0.1228(3) 0.1482(4) 0.112(3) Uani 1 1 d . . . H19A H 0.0046 0.1275 0.1788 0.168 Uiso 1 1 calc R . . H19B H 0.0003 0.0904 0.1336 0.168 Uiso 1 1 calc R . . H19C H 0.0058 0.1523 0.1275 0.168 Uiso 1 1 calc R . . C31 C -0.2304(6) 0.3392(4) 0.3562(3) 0.116(3) Uani 1 1 d . . . H31 H -0.2182 0.3120 0.3787 0.139 Uiso 1 1 calc R . . C50 C 0.5725(7) 0.5659(4) 0.2268(3) 0.106(3) Uani 1 1 d . . . H50 H 0.6274 0.5629 0.2108 0.128 Uiso 1 1 calc R . . C66 C 0.3092(5) 0.4663(3) 0.4844(3) 0.0780(18) Uani 1 1 d . . . H66 H 0.2789 0.4749 0.4536 0.094 Uiso 1 1 calc R . . C51 C 0.5010(7) 0.6020(4) 0.2116(4) 0.116(3) Uani 1 1 d . . . H51 H 0.5105 0.6279 0.1891 0.139 Uiso 1 1 calc R . . N2 N -0.2323(6) 0.6043(3) 0.1526(2) 0.103(2) Uani 1 1 d D . . C42 C 0.1760(5) 0.6583(2) 0.2761(2) 0.0692(16) Uani 1 1 d . . . H42 H 0.2001 0.6694 0.3073 0.083 Uiso 1 1 calc R . . N3 N 0.4050(6) 0.6918(3) 0.4785(2) 0.106(2) Uani 1 1 d . . . N4 N 0.2520(6) 0.1576(2) 0.5573(2) 0.106(2) Uani 1 1 d . . . C17 C 0.2878(5) 0.1572(3) 0.1875(2) 0.0734(17) Uani 1 1 d . . . H17 H 0.3186 0.1255 0.1811 0.088 Uiso 1 1 calc R . . C44 C 0.0771(5) 0.6754(3) 0.2029(3) 0.085(2) Uani 1 1 d . . . H44 H 0.0329 0.6971 0.1834 0.102 Uiso 1 1 calc R . . C72 C -0.0013(5) 0.3848(3) 0.4510(3) 0.084(2) Uani 1 1 d . . . H72 H 0.0028 0.3649 0.4234 0.100 Uiso 1 1 calc R . . C80 C 0.2125(7) 0.1441(3) 0.6024(3) 0.110(3) Uani 1 1 d . . . H80A H 0.2159 0.1748 0.6229 0.166 Uiso 1 1 calc R . . H80B H 0.2511 0.1159 0.6187 0.166 Uiso 1 1 calc R . . H80C H 0.1450 0.1328 0.5948 0.166 Uiso 1 1 calc R . . C63 C 0.4088(6) 0.4392(4) 0.5725(3) 0.109(3) Uani 1 1 d . . . H63 H 0.4428 0.4298 0.6024 0.130 Uiso 1 1 calc R . . C49 C 0.5643(6) 0.5346(3) 0.2647(4) 0.107(3) Uani 1 1 d . . . H49 H 0.6183 0.5143 0.2780 0.128 Uiso 1 1 calc R . . C45 C 0.1041(7) 0.6265(3) 0.1855(3) 0.114(3) Uani 1 1 d . . . H45 H 0.0804 0.6162 0.1541 0.137 Uiso 1 1 calc R . . C64 C 0.4217(6) 0.4871(4) 0.5548(4) 0.113(3) Uani 1 1 d . . . H64 H 0.4655 0.5105 0.5724 0.135 Uiso 1 1 calc R . . C65 C 0.3709(6) 0.5033(4) 0.5104(3) 0.103(3) Uani 1 1 d . . . H65 H 0.3780 0.5375 0.4986 0.123 Uiso 1 1 calc R . . C3 C 0.6335(7) 0.2307(4) 0.3080(5) 0.124(4) Uani 1 1 d . . . H3 H 0.6939 0.2229 0.2980 0.149 Uiso 1 1 calc R . . C70 C -0.0996(7) 0.4292(4) 0.5013(4) 0.107(3) Uani 1 1 d . . . H70 H -0.1609 0.4390 0.5092 0.128 Uiso 1 1 calc R . . C4 C 0.6194(8) 0.2165(4) 0.3506(5) 0.124(4) Uani 1 1 d . . . H4 H 0.6688 0.1987 0.3706 0.149 Uiso 1 1 calc R . . C11 C 0.4950(7) 0.3384(5) 0.1290(3) 0.120(3) Uani 1 1 d . . . H11 H 0.5054 0.3226 0.1001 0.144 Uiso 1 1 calc R . . C71 C -0.0949(6) 0.4033(4) 0.4619(5) 0.126(4) Uani 1 1 d . . . H71 H -0.1522 0.3966 0.4406 0.151 Uiso 1 1 calc R . . C28 C -0.2617(7) 0.4183(4) 0.2907(3) 0.124(4) Uani 1 1 d . . . H28 H -0.2701 0.4477 0.2703 0.148 Uiso 1 1 calc R . . C69 C -0.0185(9) 0.4420(5) 0.5305(3) 0.132(4) Uani 1 1 d . . . H69 H -0.0261 0.4598 0.5588 0.159 Uiso 1 1 calc R . . C79 C 0.2819(9) 0.1130(3) 0.5329(3) 0.120(3) Uani 1 1 d . . . H79A H 0.2297 0.1025 0.5081 0.179 Uiso 1 1 calc R . . H79B H 0.2967 0.0842 0.5553 0.179 Uiso 1 1 calc R . . H79C H 0.3399 0.1217 0.5188 0.179 Uiso 1 1 calc R . . C9 C 0.5152(7) 0.4116(4) 0.1798(4) 0.119(3) Uani 1 1 d . . . H9 H 0.5373 0.4461 0.1865 0.143 Uiso 1 1 calc R . . C10 C 0.5294(7) 0.3896(4) 0.1390(4) 0.117(3) Uani 1 1 d . . . H10 H 0.5620 0.4080 0.1172 0.140 Uiso 1 1 calc R . . C29 C -0.3335(8) 0.4076(4) 0.3206(4) 0.131(4) Uani 1 1 d . . . H29 H -0.3927 0.4264 0.3169 0.157 Uiso 1 1 calc R . . C5 C 0.5249(10) 0.2286(4) 0.3672(4) 0.136(4) Uani 1 1 d . . . H5 H 0.5138 0.2195 0.3981 0.163 Uiso 1 1 calc R . . C60 C 0.4848(9) 0.7262(5) 0.4826(4) 0.169(6) Uani 1 1 d . . . H60A H 0.5336 0.7127 0.4642 0.253 Uiso 1 1 calc R . . H60B H 0.5131 0.7291 0.5159 0.253 Uiso 1 1 calc R . . H60C H 0.4631 0.7606 0.4706 0.253 Uiso 1 1 calc R . . C59 C 0.3734(11) 0.6740(6) 0.5233(4) 0.196(7) Uani 1 1 d . . . H59A H 0.3025 0.6730 0.5196 0.295 Uiso 1 1 calc R . . H59B H 0.3976 0.6982 0.5488 0.295 Uiso 1 1 calc R . . H59C H 0.3993 0.6390 0.5312 0.295 Uiso 1 1 calc R . . C25 C -0.0844(5) 0.2922(3) 0.1396(2) 0.101(3) Uani 1 1 d . . . H25 H -0.0375 0.2808 0.1208 0.121 Uiso 1 1 calc R . . C39 C -0.3207(5) 0.6019(3) 0.1126(2) 0.343(18) Uani 1 1 d RD . . H39A H -0.3285 0.6356 0.0965 0.515 Uiso 1 1 calc R . . H39B H -0.3794 0.5937 0.1264 0.515 Uiso 1 1 calc R . . H39C H -0.3098 0.5747 0.0899 0.515 Uiso 1 1 calc R . . C40 C -0.2101(10) 0.6529(3) 0.1754(5) 0.198(8) Uani 1 1 d D . . H40A H -0.2153 0.6496 0.2091 0.297 Uiso 1 1 calc R . . H40B H -0.2558 0.6795 0.1612 0.297 Uiso 1 1 calc R . . H40C H -0.1440 0.6633 0.1717 0.297 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0557(2) 0.04079(19) 0.0582(2) -0.00321(14) 0.00658(15) -0.00187(14) I2 0.0657(2) 0.0554(2) 0.0536(2) -0.00576(15) 0.01320(16) -0.00345(16) I3 0.05178(19) 0.0484(2) 0.0543(2) -0.00381(14) 0.01068(14) 0.00554(14) I4 0.04569(18) 0.0546(2) 0.0557(2) -0.00765(15) 0.00855(14) -0.00525(14) Cu2 0.0529(4) 0.0623(4) 0.0688(5) -0.0018(3) 0.0033(3) 0.0025(3) Cu4 0.0669(4) 0.0626(4) 0.0525(4) -0.0031(3) 0.0145(3) -0.0053(3) Cu3 0.0757(5) 0.0553(4) 0.0703(5) -0.0037(3) 0.0209(4) -0.0149(4) P4 0.0577(8) 0.0491(7) 0.0459(7) -0.0039(6) 0.0086(6) -0.0009(6) P2 0.0473(7) 0.0475(7) 0.0589(8) 0.0025(6) 0.0045(6) 0.0013(6) P1 0.0574(8) 0.0552(8) 0.0642(9) -0.0152(7) 0.0076(6) 0.0000(7) P3 0.0521(7) 0.0471(7) 0.0518(7) 0.0006(6) 0.0094(6) -0.0050(6) Cu1 0.0694(5) 0.0622(4) 0.0726(5) -0.0179(4) 0.0135(4) 0.0005(4) C53 0.063(3) 0.040(3) 0.055(3) 0.003(2) 0.011(2) -0.002(2) C33 0.058(3) 0.048(3) 0.050(3) 0.001(2) 0.011(2) 0.003(2) C15 0.054(3) 0.065(4) 0.069(4) -0.017(3) 0.003(3) 0.005(3) C27 0.060(3) 0.057(3) 0.056(3) 0.004(3) 0.007(2) -0.002(3) C73 0.065(3) 0.054(3) 0.049(3) 0.001(2) 0.011(2) 0.005(3) C13 0.064(3) 0.055(3) 0.058(3) -0.006(2) 0.009(2) 0.001(3) C47 0.055(3) 0.045(3) 0.061(3) 0.000(2) 0.016(2) 0.003(2) C1 0.065(4) 0.062(4) 0.081(4) -0.021(3) -0.007(3) 0.005(3) C14 0.052(3) 0.068(4) 0.063(3) -0.014(3) 0.004(2) 0.011(3) C41 0.051(3) 0.047(3) 0.067(3) -0.002(2) 0.009(2) 0.002(2) N1 0.080(4) 0.065(4) 0.097(4) -0.023(3) 0.001(3) -0.017(3) C74 0.097(5) 0.062(4) 0.059(4) 0.004(3) 0.026(3) 0.009(3) C16 0.072(4) 0.066(4) 0.054(3) -0.008(3) 0.005(3) -0.009(3) C78 0.085(4) 0.060(3) 0.045(3) -0.001(2) 0.013(3) 0.000(3) C58 0.075(4) 0.058(3) 0.059(3) 0.001(3) 0.016(3) -0.014(3) C67 0.058(3) 0.059(3) 0.060(3) 0.002(3) 0.017(3) 0.013(3) C7 0.055(3) 0.065(4) 0.082(4) -0.008(3) 0.012(3) -0.010(3) C77 0.102(5) 0.048(3) 0.060(4) -0.007(3) 0.016(3) 0.011(3) C22 0.062(4) 0.071(4) 0.081(4) -0.006(3) 0.001(3) -0.014(3) C61 0.056(3) 0.066(4) 0.065(4) -0.013(3) 0.000(3) 0.001(3) C48 0.066(4) 0.066(4) 0.125(6) 0.018(4) 0.030(4) 0.005(3) C18 0.057(3) 0.052(3) 0.086(4) -0.020(3) 0.007(3) 0.007(3) C21 0.059(3) 0.055(3) 0.061(3) 0.000(3) -0.001(3) 0.003(3) C75 0.101(5) 0.070(4) 0.060(4) 0.001(3) 0.020(3) 0.006(4) C57 0.063(4) 0.085(5) 0.081(5) -0.009(4) 0.011(3) -0.026(3) C68 0.091(5) 0.096(5) 0.070(4) -0.017(4) 0.016(4) 0.010(4) C38 0.070(4) 0.060(4) 0.073(4) 0.008(3) -0.002(3) -0.012(3) C76 0.095(5) 0.059(4) 0.061(4) 0.008(3) -0.001(3) -0.007(3) C46 0.125(7) 0.070(4) 0.076(5) -0.005(4) -0.024(4) 0.014(4) C36 0.080(4) 0.060(4) 0.067(4) 0.017(3) 0.023(3) 0.016(3) C34 0.075(4) 0.062(4) 0.084(5) 0.009(3) -0.012(3) 0.006(3) C20 0.102(6) 0.092(6) 0.091(6) -0.018(4) 0.004(4) -0.021(5) C32 0.077(4) 0.086(5) 0.095(5) 0.035(4) 0.019(4) 0.002(4) C56 0.101(5) 0.065(4) 0.057(4) -0.007(3) 0.003(3) -0.024(4) C12 0.109(6) 0.071(4) 0.079(5) -0.014(4) 0.033(4) -0.004(4) C43 0.070(4) 0.080(5) 0.097(6) 0.018(4) 0.010(4) 0.007(4) C55 0.157(8) 0.114(6) 0.058(4) -0.019(4) 0.037(5) -0.058(6) C26 0.070(4) 0.074(4) 0.081(4) -0.024(3) 0.001(3) 0.008(3) C23 0.091(5) 0.055(4) 0.105(6) -0.013(4) -0.010(4) -0.014(4) C35 0.096(5) 0.042(3) 0.096(5) 0.008(3) 0.000(4) -0.009(3) C62 0.093(5) 0.068(4) 0.095(5) -0.002(4) -0.022(4) -0.004(4) C52 0.077(5) 0.124(7) 0.102(6) 0.056(5) 0.033(4) 0.014(4) C8 0.102(6) 0.066(4) 0.106(6) -0.017(4) 0.036(5) -0.020(4) C37 0.082(5) 0.092(5) 0.064(4) 0.010(4) -0.012(3) 0.014(4) C6 0.103(6) 0.071(4) 0.077(5) -0.010(4) -0.013(4) 0.004(4) C2 0.072(5) 0.091(5) 0.107(6) -0.016(4) -0.007(4) 0.001(4) C30 0.085(6) 0.169(9) 0.076(5) 0.027(5) 0.025(4) -0.013(6) C24 0.115(6) 0.058(4) 0.104(6) -0.019(4) -0.032(5) 0.002(4) C54 0.121(6) 0.082(5) 0.065(4) -0.018(3) 0.030(4) -0.040(4) C19 0.083(6) 0.092(6) 0.161(9) -0.044(6) 0.020(5) -0.015(5) C31 0.086(6) 0.163(9) 0.101(6) 0.065(6) 0.021(5) 0.008(6) C50 0.104(7) 0.106(7) 0.124(7) -0.004(5) 0.066(6) -0.006(5) C66 0.077(4) 0.076(5) 0.079(4) -0.009(3) 0.004(3) -0.008(3) C51 0.096(6) 0.142(8) 0.124(7) 0.040(6) 0.066(6) 0.029(6) N2 0.125(6) 0.103(6) 0.078(5) 0.012(4) 0.000(4) 0.046(5) C42 0.076(4) 0.059(4) 0.072(4) -0.008(3) 0.007(3) 0.012(3) N3 0.167(7) 0.081(4) 0.071(4) -0.012(3) 0.017(4) -0.053(4) N4 0.177(7) 0.069(4) 0.074(4) 0.015(3) 0.019(4) 0.037(4) C17 0.069(4) 0.063(4) 0.085(5) -0.022(3) 0.003(3) 0.008(3) C44 0.083(5) 0.070(5) 0.094(5) 0.022(4) -0.011(4) -0.004(4) C72 0.068(4) 0.075(5) 0.112(6) -0.025(4) 0.030(4) -0.015(3) C80 0.144(8) 0.080(5) 0.106(6) 0.042(5) 0.014(5) -0.036(5) C63 0.090(6) 0.114(7) 0.107(7) -0.032(5) -0.039(5) 0.024(5) C49 0.072(5) 0.066(5) 0.189(10) 0.019(5) 0.043(5) 0.007(4) C45 0.151(8) 0.089(6) 0.086(6) -0.011(4) -0.041(5) 0.019(5) C64 0.088(6) 0.100(7) 0.139(8) -0.029(6) -0.020(5) -0.038(5) C65 0.088(6) 0.107(6) 0.109(7) -0.004(5) 0.002(5) -0.032(5) C3 0.077(6) 0.105(7) 0.176(11) -0.031(7) -0.034(7) 0.038(5) C70 0.094(7) 0.091(6) 0.149(9) 0.009(6) 0.064(6) 0.006(5) C4 0.111(8) 0.098(7) 0.143(10) -0.017(7) -0.051(7) 0.014(6) C11 0.122(8) 0.161(10) 0.084(6) 0.001(6) 0.038(5) 0.027(7) C71 0.059(5) 0.148(9) 0.176(11) -0.022(8) 0.032(6) -0.031(5) C28 0.129(7) 0.139(8) 0.121(7) 0.067(6) 0.079(6) 0.077(6) C69 0.159(10) 0.163(10) 0.082(6) -0.001(6) 0.042(6) 0.095(8) C79 0.201(11) 0.060(5) 0.098(6) 0.014(4) 0.022(6) 0.016(6) C9 0.122(8) 0.113(7) 0.130(8) -0.023(6) 0.043(6) -0.047(6) C10 0.112(7) 0.123(8) 0.126(8) -0.006(6) 0.053(6) -0.044(6) C29 0.134(8) 0.123(7) 0.154(9) 0.069(7) 0.086(7) 0.056(6) C5 0.204(12) 0.093(6) 0.089(6) -0.019(5) -0.057(7) 0.011(7) C60 0.149(10) 0.224(14) 0.129(9) -0.090(10) 0.003(7) -0.055(10) C59 0.295(18) 0.221(14) 0.084(7) -0.060(8) 0.064(9) -0.131(13) C25 0.119(7) 0.094(6) 0.087(6) -0.021(4) 0.006(5) 0.015(5) C39 0.70(5) 0.058(6) 0.38(3) -0.028(11) 0.45(3) -0.018(14) C40 0.194(13) 0.073(6) 0.287(18) 0.072(9) -0.105(12) -0.035(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 I1 Cu4 2.6513(8) . ? I1 Cu2 2.6962(9) . ? I1 Cu1 2.7410(9) . ? I2 Cu2 2.6703(9) . ? I2 Cu1 2.6859(10) . ? I2 Cu3 2.6919(9) . ? I3 Cu3 2.6280(9) . ? I3 Cu2 2.7029(9) . ? I3 Cu4 2.7831(9) . ? I4 Cu1 2.6567(9) . ? I4 Cu4 2.6738(8) . ? I4 Cu3 2.8261(9) . ? Cu2 P2 2.2522(16) . ? Cu2 Cu1 3.0409(11) . ? Cu4 P4 2.2378(16) . ? Cu3 P3 2.2476(16) . ? P4 C61 1.822(6) . ? P4 C67 1.829(5) . ? P4 C73 1.832(6) . ? P2 C33 1.803(5) . ? P2 C21 1.827(6) . ? P2 C27 1.830(6) . ? P1 C13 1.796(6) . ? P1 C7 1.809(6) . ? P1 C1 1.824(7) . ? P1 Cu1 2.2509(16) . ? P3 C53 1.825(6) . ? P3 C47 1.827(5) . ? P3 C41 1.837(6) . ? C53 C58 1.354(8) . ? C53 C54 1.391(8) . ? C33 C38 1.374(8) . ? C33 C34 1.421(8) . ? C15 C14 1.379(8) . ? C15 C16 1.392(8) . ? C27 C28 1.325(9) . ? C27 C32 1.357(8) . ? C73 C74 1.375(8) . ? C73 C78 1.383(8) . ? C13 C14 1.396(8) . ? C13 C18 1.403(8) . ? C47 C52 1.343(8) . ? C47 C48 1.380(8) . ? C1 C2 1.382(10) . ? C1 C6 1.395(10) . ? C41 C46 1.360(9) . ? C41 C42 1.387(8) . ? N1 C16 1.373(8) . ? N1 C19 1.398(9) . ? N1 C20 1.416(9) . ? C74 C75 1.346(9) . ? C16 C17 1.357(8) . ? C78 C77 1.379(8) . ? C58 C57 1.391(9) . ? C67 C72 1.387(9) . ? C67 C68 1.419(9) . ? C7 C12 1.399(9) . ? C7 C8 1.411(9) . ? C77 C76 1.377(9) . ? C22 C23 1.340(9) . ? C22 C21 1.405(8) . ? C61 C62 1.363(9) . ? C61 C66 1.380(9) . ? C48 C49 1.397(10) . ? C18 C17 1.396(8) . ? C21 C26 1.381(9) . ? C75 C76 1.464(9) . ? C57 C56 1.384(9) . ? C68 C69 1.349(12) . ? C38 C37 1.397(9) . ? C76 N4 1.353(8) . ? C46 C45 1.384(10) . ? C36 C35 1.343(9) . ? C36 C37 1.401(10) . ? C36 N2 1.414(9) . ? C34 C35 1.355(9) . ? C32 C31 1.389(10) . ? C56 C55 1.355(9) . ? C56 N3 1.368(8) . ? C12 C11 1.391(12) . ? C43 C44 1.320(10) . ? C43 C42 1.381(9) . ? C55 C54 1.394(10) . ? C26 C25 1.415(9) . ? C23 C24 1.411(12) . ? C62 C63 1.412(11) . ? C52 C51 1.422(10) . ? C8 C9 1.348(11) . ? C6 C5 1.406(12) . ? C2 C3 1.412(12) . ? C30 C29 1.340(12) . ? C30 C31 1.394(12) . ? C24 C25 1.330(10) . ? C50 C49 1.339(12) . ? C50 C51 1.356(12) . ? C66 C65 1.389(10) . ? N2 C40 1.394(8) . ? N2 C39 1.527(7) . ? N3 C60 1.383(12) . ? N3 C59 1.456(12) . ? N4 C79 1.405(10) . ? N4 C80 1.480(10) . ? C44 C45 1.392(11) . ? C72 C71 1.434(11) . ? C63 C64 1.321(13) . ? C64 C65 1.398(13) . ? C3 C4 1.284(15) . ? C70 C71 1.290(13) . ? C70 C69 1.320(14) . ? C4 C5 1.465(16) . ? C11 C10 1.386(14) . ? C28 C29 1.404(11) . ? C9 C10 1.307(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 Cu4 I1 Cu2 75.44(3) . . ? Cu4 I1 Cu1 71.69(2) . . ? Cu2 I1 Cu1 68.01(3) . . ? Cu2 I2 Cu1 69.19(3) . . ? Cu2 I2 Cu3 71.17(3) . . ? Cu1 I2 Cu3 73.22(3) . . ? Cu3 I3 Cu2 71.63(2) . . ? Cu3 I3 Cu4 77.75(3) . . ? Cu2 I3 Cu4 73.21(2) . . ? Cu1 I4 Cu4 72.67(3) . . ? Cu1 I4 Cu3 71.52(3) . . ? Cu4 I4 Cu3 76.26(3) . . ? P2 Cu2 I2 112.58(5) . . ? P2 Cu2 I1 115.52(5) . . ? I2 Cu2 I1 109.73(3) . . ? P2 Cu2 I3 108.96(5) . . ? I2 Cu2 I3 106.06(3) . . ? I1 Cu2 I3 103.13(3) . . ? P2 Cu2 Cu1 149.71(5) . . ? I2 Cu2 Cu1 55.65(2) . . ? I1 Cu2 Cu1 56.70(2) . . ? I3 Cu2 Cu1 101.30(3) . . ? P4 Cu4 I1 121.02(5) . . ? P4 Cu4 I4 117.24(5) . . ? I1 Cu4 I4 106.84(3) . . ? P4 Cu4 I3 105.81(4) . . ? I1 Cu4 I3 102.16(3) . . ? I4 Cu4 I3 100.64(3) . . ? P3 Cu3 I3 117.92(5) . . ? P3 Cu3 I2 111.74(5) . . ? I3 Cu3 I2 107.60(3) . . ? P3 Cu3 I4 114.93(5) . . ? I3 Cu3 I4 100.67(3) . . ? I2 Cu3 I4 102.35(3) . . ? C61 P4 C67 103.7(3) . . ? C61 P4 C73 105.2(3) . . ? C67 P4 C73 102.6(3) . . ? C61 P4 Cu4 113.3(2) . . ? C67 P4 Cu4 111.28(19) . . ? C73 P4 Cu4 119.18(18) . . ? C33 P2 C21 102.6(3) . . ? C33 P2 C27 103.2(3) . . ? C21 P2 C27 103.1(3) . . ? C33 P2 Cu2 115.46(19) . . ? C21 P2 Cu2 116.24(19) . . ? C27 P2 Cu2 114.43(19) . . ? C13 P1 C7 104.3(3) . . ? C13 P1 C1 104.0(3) . . ? C7 P1 C1 103.7(3) . . ? C13 P1 Cu1 114.9(2) . . ? C7 P1 Cu1 113.7(2) . . ? C1 P1 Cu1 115.0(2) . . ? C53 P3 C47 102.5(3) . . ? C53 P3 C41 102.4(2) . . ? C47 P3 C41 102.9(2) . . ? C53 P3 Cu3 117.35(17) . . ? C47 P3 Cu3 112.67(18) . . ? C41 P3 Cu3 117.02(18) . . ? P1 Cu1 I4 114.78(5) . . ? P1 Cu1 I2 109.55(5) . . ? I4 Cu1 I2 107.18(3) . . ? P1 Cu1 I1 112.26(5) . . ? I4 Cu1 I1 104.78(3) . . ? I2 Cu1 I1 107.93(3) . . ? P1 Cu1 Cu2 141.51(5) . . ? I4 Cu1 Cu2 103.70(3) . . ? I2 Cu1 Cu2 55.16(2) . . ? I1 Cu1 Cu2 55.30(2) . . ? C58 C53 C54 117.6(5) . . ? C58 C53 P3 124.0(4) . . ? C54 C53 P3 118.4(4) . . ? C38 C33 C34 115.7(5) . . ? C38 C33 P2 125.0(4) . . ? C34 C33 P2 119.2(4) . . ? C14 C15 C16 122.2(5) . . ? C28 C27 C32 118.9(6) . . ? C28 C27 P2 123.8(5) . . ? C32 C27 P2 117.2(5) . . ? C74 C73 C78 117.3(5) . . ? C74 C73 P4 123.5(4) . . ? C78 C73 P4 119.2(4) . . ? C14 C13 C18 115.8(5) . . ? C14 C13 P1 119.5(4) . . ? C18 C13 P1 124.5(4) . . ? C52 C47 C48 118.6(6) . . ? C52 C47 P3 123.7(5) . . ? C48 C47 P3 117.7(5) . . ? C2 C1 C6 119.4(7) . . ? C2 C1 P1 123.8(6) . . ? C6 C1 P1 116.8(5) . . ? C15 C14 C13 121.7(5) . . ? C46 C41 C42 117.8(6) . . ? C46 C41 P3 118.5(5) . . ? C42 C41 P3 123.7(5) . . ? C16 N1 C19 121.9(6) . . ? C16 N1 C20 119.9(6) . . ? C19 N1 C20 115.3(6) . . ? C75 C74 C73 124.3(6) . . ? C17 C16 N1 123.3(6) . . ? C17 C16 C15 116.3(5) . . ? N1 C16 C15 120.4(6) . . ? C77 C78 C73 120.8(5) . . ? C53 C58 C57 122.4(6) . . ? C72 C67 C68 118.9(6) . . ? C72 C67 P4 117.4(5) . . ? C68 C67 P4 123.3(5) . . ? C12 C7 C8 115.8(6) . . ? C12 C7 P1 124.6(5) . . ? C8 C7 P1 119.6(5) . . ? C76 C77 C78 122.6(6) . . ? C23 C22 C21 121.4(7) . . ? C62 C61 C66 118.9(6) . . ? C62 C61 P4 124.3(5) . . ? C66 C61 P4 116.7(5) . . ? C47 C48 C49 119.2(7) . . ? C17 C18 C13 121.0(6) . . ? C26 C21 C22 120.6(6) . . ? C26 C21 P2 116.6(5) . . ? C22 C21 P2 122.8(5) . . ? C74 C75 C76 118.8(6) . . ? C56 C57 C58 120.7(6) . . ? C69 C68 C67 115.9(8) . . ? C33 C38 C37 122.7(6) . . ? N4 C76 C77 124.1(7) . . ? N4 C76 C75 119.6(6) . . ? C77 C76 C75 116.2(6) . . ? C41 C46 C45 120.6(7) . . ? C35 C36 C37 117.1(6) . . ? C35 C36 N2 122.4(7) . . ? C37 C36 N2 120.5(7) . . ? C35 C34 C33 120.4(6) . . ? C27 C32 C31 120.1(7) . . ? C55 C56 N3 122.6(7) . . ? C55 C56 C57 116.5(6) . . ? N3 C56 C57 120.9(6) . . ? C11 C12 C7 118.7(8) . . ? C44 C43 C42 119.4(7) . . ? C56 C55 C54 123.6(7) . . ? C21 C26 C25 115.5(6) . . ? C22 C23 C24 119.4(7) . . ? C36 C35 C34 124.4(6) . . ? C61 C62 C63 119.5(8) . . ? C47 C52 C51 122.0(7) . . ? C9 C8 C7 122.9(8) . . ? C36 C37 C38 119.7(6) . . ? C1 C6 C5 120.0(9) . . ? C1 C2 C3 119.7(10) . . ? C29 C30 C31 118.6(7) . . ? C25 C24 C23 118.5(7) . . ? C53 C54 C55 119.2(6) . . ? C32 C31 C30 120.2(8) . . ? C49 C50 C51 120.2(7) . . ? C61 C66 C65 121.7(7) . . ? C50 C51 C52 117.8(8) . . ? C40 N2 C36 122.5(7) . . ? C40 N2 C39 118.0(7) . . ? C36 N2 C39 116.7(7) . . ? C43 C42 C41 121.9(7) . . ? C56 N3 C60 120.9(8) . . ? C56 N3 C59 119.5(7) . . ? C60 N3 C59 116.5(8) . . ? C76 N4 C79 122.0(7) . . ? C76 N4 C80 123.3(7) . . ? C79 N4 C80 113.5(7) . . ? C16 C17 C18 122.9(6) . . ? C43 C44 C45 120.8(7) . . ? C67 C72 C71 118.4(8) . . ? C64 C63 C62 120.7(8) . . ? C50 C49 C48 121.3(8) . . ? C46 C45 C44 119.5(7) . . ? C63 C64 C65 121.6(7) . . ? C66 C65 C64 117.2(8) . . ? C4 C3 C2 123.1(11) . . ? C71 C70 C69 120.9(9) . . ? C3 C4 C5 119.5(10) . . ? C10 C11 C12 122.1(9) . . ? C70 C71 C72 119.9(10) . . ? C27 C28 C29 122.3(7) . . ? C70 C69 C68 125.1(9) . . ? C10 C9 C8 121.6(9) . . ? C9 C10 C11 118.8(9) . . ? C30 C29 C28 119.2(8) . . ? C6 C5 C4 118.3(11) . . ? C24 C25 C26 124.4(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.027 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.142 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.056 0.500 0.000 1041.2 36.3 2 0.005 1.000 0.500 1041.1 36.6 3 0.242 0.979 0.095 9.3 -0.2 4 0.242 0.521 0.595 9.3 0.0 5 0.757 0.479 0.405 9.3 -0.3 6 0.757 0.021 0.905 9.3 0.3 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 928676'