# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Michael Hannon' 'Nathaniel J. Alcock' 'Guy Clarkson' 'Arnaud Lavalette' 'Floriana Tuna' _publ_contact_author_name 'Dr Michael Hannon' _publ_contact_author_address ; Department of Chemistry University of Warwick Coventry CV4 7AL UNITED KINGDOM ; _publ_contact_author_email M.J.HANNON@WARWICK.AC.UK _publ_section_title ; Aggregation of metallo-supramolecular architectures by metallo-assembled hydrogen bonding sites ; data_al1 _database_code_CSD 211775 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H60 Cu2 F12 N12 O4 P2' _chemical_formula_weight 1454.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _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 8.633(2) _cell_length_b 14.567(4) _cell_length_c 14.634(4) _cell_angle_alpha 80.887(6) _cell_angle_beta 75.750(7) _cell_angle_gamma 77.550(5) _cell_volume 1730.9(8) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1853 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 7169 _diffrn_reflns_av_R_equivalents 0.0882 _diffrn_reflns_av_sigmaI/netI 0.2144 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4469 _reflns_number_gt 2017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0058(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4469 _refine_ls_number_parameters 434 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1744 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1424 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.80358(15) 0.76021(8) -0.76770(7) 0.0397(5) Uani 1 1 d . . . C2 C 0.8323(14) 0.1906(7) -0.1485(7) 0.059(3) Uani 1 1 d . . . H2A H 0.9009 0.1781 -0.1011 0.071 Uiso 0.731(16) 1 calc PR A 1 H2B H 0.8191 0.2591 -0.1707 0.071 Uiso 0.731(16) 1 calc PR A 1 H2C H 0.8797 0.2475 -0.1516 0.071 Uiso 0.269(16) 1 d PR A 2 H2D H 0.7152 0.2112 -0.1484 0.071 Uiso 0.269(16) 1 d PR A 2 O1 O 0.6775(13) 0.1702(7) -0.1022(6) 0.077(5) Uani 0.731(16) 1 d P A 1 H1 H 0.6051 0.2141 -0.1181 0.115 Uiso 0.731(16) 1 calc PR A 1 O1A O 0.848(3) 0.1365(16) -0.0696(16) 0.055(11) Uiso 0.269(16) 1 d P A 2 H1A H 0.9252 0.1485 -0.0504 0.082 Uiso 0.269(16) 1 calc PR A 2 C3 C 0.9204(14) 0.1386(7) -0.2295(7) 0.041(3) Uani 1 1 d . A . N4 N 1.0711(10) 0.1535(5) -0.2672(5) 0.035(2) Uani 1 1 d . . . C5 C 1.1590(12) 0.1074(6) -0.3407(7) 0.034(2) Uani 1 1 d . A . C6 C 1.1030(13) 0.0443(6) -0.3801(7) 0.049(3) Uani 1 1 d . . . H6A H 1.1684 0.0129 -0.4325 0.058 Uiso 1 1 calc R A . C7 C 0.9444(15) 0.0290(7) -0.3389(8) 0.057(3) Uani 1 1 d . A . H7A H 0.8994 -0.0129 -0.3641 0.068 Uiso 1 1 calc R . . C8 C 0.8553(12) 0.0737(7) -0.2630(7) 0.049(3) Uani 1 1 d . . . H8A H 0.7499 0.0612 -0.2330 0.059 Uiso 1 1 calc R A . C9 C 1.3227(11) 0.1274(6) -0.3803(6) 0.028(2) Uani 1 1 d . . . H9A H 1.3921 0.0970 -0.4324 0.033 Uiso 1 1 calc R A . N10 N 1.3697(8) 0.1873(5) -0.3424(4) 0.0295(19) Uani 1 1 d . . . C11 C 1.5277(11) 0.2119(6) -0.3810(6) 0.029(2) Uani 1 1 d . . . C12 C 1.6336(11) 0.1814(6) -0.4630(6) 0.035(2) Uani 1 1 d . A . H12A H 1.6067 0.1391 -0.4972 0.042 Uiso 1 1 calc R . . C13 C 1.7790(12) 0.2139(6) -0.4941(6) 0.040(3) Uani 1 1 d . . . H13A H 1.8512 0.1934 -0.5504 0.048 Uiso 1 1 calc R A . C14 C 1.8238(11) 0.2764(6) -0.4452(6) 0.030(2) Uani 1 1 d . A . C15 C 1.7210(12) 0.3050(6) -0.3632(6) 0.034(2) Uani 1 1 d . . . H15A H 1.7506 0.3459 -0.3286 0.041 Uiso 1 1 calc R A . C16 C 1.5718(12) 0.2739(6) -0.3303(6) 0.035(2) Uani 1 1 d . A . H16A H 1.5001 0.2946 -0.2739 0.042 Uiso 1 1 calc R . . C17 C 1.9791(7) 0.3149(4) -0.4858(4) 0.042(3) Uani 1 1 d . . . H17A H 2.0667 0.2637 -0.5120 0.051 Uiso 1 1 calc R A . H17B H 2.0126 0.3376 -0.4347 0.051 Uiso 1 1 calc R . . C18 C 1.9556(7) 0.3969(4) -0.5648(4) 0.035(2) Uani 1 1 d R A . C19 C 1.8392(7) 0.4770(4) -0.5425(4) 0.039(2) Uani 1 1 d R . . H19A H 1.7788 0.4815 -0.4791 0.047 Uiso 1 1 calc R . . C20 C 1.8111(11) 0.5514(6) -0.6136(6) 0.035(2) Uani 1 1 d . A . H20A H 1.7344 0.6072 -0.5981 0.042 Uiso 1 1 calc R . . C21 C 1.8955(11) 0.5433(6) -0.7067(6) 0.030(2) Uani 1 1 d . . . C22 C 2.0097(13) 0.4647(7) -0.7278(6) 0.050(3) Uani 1 1 d . A . H22A H 2.0686 0.4596 -0.7914 0.060 Uiso 1 1 calc R . . C23 C 2.0412(12) 0.3915(6) -0.6572(7) 0.049(3) Uani 1 1 d . . . H23A H 2.1223 0.3375 -0.6730 0.059 Uiso 1 1 calc R A . N24 N 1.8565(9) 0.6192(5) -0.7773(5) 0.0339(19) Uani 1 1 d . A . C25 C 1.8471(12) 0.5997(7) -0.8578(7) 0.049(3) Uani 1 1 d . . . H25A H 1.8678 0.5360 -0.8713 0.059 Uiso 1 1 calc R A . C26 C 1.8049(13) 0.6756(8) -0.9266(6) 0.052(3) Uani 1 1 d . A . N27 N 1.7747(9) 0.7623(6) -0.9011(5) 0.038(2) Uani 1 1 d . . . C28 C 1.7316(11) 0.8375(7) -0.9634(7) 0.046(3) Uani 1 1 d . A . C29 C 1.7035(14) 0.9316(7) -0.9299(7) 0.069(3) Uani 1 1 d . . . H29A H 1.6137 0.9350 -0.8728 0.082 Uiso 1 1 calc R A . H29B H 1.8025 0.9390 -0.9112 0.082 Uiso 1 1 calc R . . O30 O 1.6664(12) 1.0037(5) -0.9955(5) 0.122(3) Uani 1 1 d . A . H30 H 1.7074 1.0496 -0.9908 0.183 Uiso 1 1 calc R . . C31 C 1.7217(15) 0.8238(9) -1.0533(7) 0.079(4) Uani 1 1 d . . . H31A H 1.6907 0.8769 -1.0961 0.095 Uiso 1 1 calc R A . C32 C 1.7545(12) 0.7384(7) -1.0802(6) 0.109(6) Uani 1 1 d . A . H32D H 1.7512 0.7296 -1.1426 0.131 Uiso 1 1 calc R . . C33 C 1.7941(12) 0.6611(7) -1.0157(6) 0.085(4) Uani 1 1 d R . . H33A H 1.8131 0.5980 -1.0327 0.102 Uiso 1 1 d R . . P1 P 1.5915(3) -0.13108(18) -0.32251(18) 0.0451(8) Uani 1 1 d . . . F1 F 1.6401(7) -0.2033(4) -0.4023(4) 0.0643(17) Uani 1 1 d . . . F2 F 1.5478(8) -0.0602(4) -0.2462(4) 0.086(2) Uani 1 1 d . . . F3 F 1.7735(7) -0.1583(4) -0.3069(4) 0.0693(18) Uani 1 1 d . . . F4 F 1.6417(7) -0.0487(3) -0.4030(3) 0.0624(17) Uani 1 1 d . . . F5 F 1.4096(6) -0.1049(4) -0.3397(3) 0.0653(17) Uani 1 1 d . . . F6 F 1.5430(8) -0.2148(4) -0.2449(4) 0.082(2) Uani 1 1 d . . . N100 N 1.517(2) 0.4871(12) -0.2175(11) 0.150(7) Uani 1 1 d . . . C101 C 1.487(2) 0.5444(15) -0.2782(15) 0.114(6) Uani 1 1 d . . . C102 C 1.459(2) 0.6081(11) -0.3577(11) 0.132(6) Uani 1 1 d . . . H10A H 1.5534 0.6391 -0.3839 0.197 Uiso 1 1 calc R . . H10B H 1.3622 0.6560 -0.3387 0.197 Uiso 1 1 calc R . . H10C H 1.4428 0.5738 -0.4059 0.197 Uiso 1 1 calc R . . N200 N 0.820(3) 0.4242(14) -0.0001(13) 0.085(7) Uiso 0.475(10) 1 d P B 1 C201 C 0.710(3) 0.3932(13) 0.0071(12) 0.040(6) Uiso 0.475(10) 1 d P B 1 C202 C 0.568(3) 0.3623(14) 0.0229(14) 0.064(7) Uiso 0.475(10) 1 d P B 1 H20B H 0.5817 0.3105 -0.0155 0.096 Uiso 0.475(10) 1 calc PR B 1 H20C H 0.4839 0.4143 0.0054 0.096 Uiso 0.475(10) 1 calc PR B 1 H20D H 0.5355 0.3395 0.0902 0.096 Uiso 0.475(10) 1 calc PR B 1 N300 N 0.900(4) 0.167(3) 0.158(2) 0.009(11) Uiso 0.182(13) 1 d P C 2 C301 C 0.827(7) 0.214(4) 0.139(4) 0.048(18) Uiso 0.182(13) 1 d P C 2 C302 C 0.780(5) 0.268(3) 0.067(3) 0.023(14) Uiso 0.182(13) 1 d P C 2 H30A H 0.6855 0.3156 0.0905 0.034 Uiso 0.182(13) 1 calc PR C 2 H30B H 0.7501 0.2290 0.0276 0.034 Uiso 0.182(13) 1 calc PR C 2 H30C H 0.8687 0.2989 0.0298 0.034 Uiso 0.182(13) 1 calc PR C 2 N400 N 0.907(4) 0.101(2) 0.098(2) 0.123(15) Uiso 0.428(13) 1 d P D 3 C401 C 0.866(4) 0.132(3) 0.135(3) 0.069(11) Uiso 0.428(13) 1 d P D 3 C402 C 0.883(3) 0.2177(16) 0.2059(17) 0.057(8) Uiso 0.428(13) 1 d P D 3 H40A H 0.7773 0.2384 0.2471 0.086 Uiso 0.428(13) 1 calc PR D 3 H40B H 0.9197 0.2723 0.1644 0.086 Uiso 0.428(13) 1 calc PR D 3 H40C H 0.9627 0.1892 0.2449 0.086 Uiso 0.428(13) 1 calc PR D 3 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 Cu1 0.0432(9) 0.0400(8) 0.0361(8) 0.0028(5) -0.0101(6) -0.0118(6) C2 0.047(9) 0.064(8) 0.057(8) 0.013(7) -0.005(7) -0.014(6) O1 0.055(9) 0.080(8) 0.074(8) -0.002(6) 0.019(6) -0.011(6) C3 0.047(8) 0.038(6) 0.036(6) 0.011(5) -0.011(6) -0.012(6) N4 0.030(6) 0.034(5) 0.035(5) 0.011(4) -0.006(4) -0.008(4) C5 0.040(7) 0.020(5) 0.046(7) 0.013(5) -0.021(6) -0.012(5) C6 0.047(8) 0.044(7) 0.060(7) 0.006(5) -0.021(6) -0.018(6) C7 0.055(9) 0.053(7) 0.073(9) 0.022(6) -0.040(7) -0.024(7) C8 0.023(7) 0.051(7) 0.064(8) 0.017(6) -0.004(6) -0.012(6) C9 0.027(6) 0.026(5) 0.030(5) 0.007(4) -0.015(5) -0.002(5) N10 0.028(5) 0.034(5) 0.030(4) 0.009(4) -0.017(4) -0.012(4) C11 0.019(6) 0.030(6) 0.039(6) 0.008(5) -0.018(5) -0.002(5) C12 0.036(7) 0.027(5) 0.045(6) -0.008(5) -0.009(5) -0.012(5) C13 0.041(7) 0.037(6) 0.038(6) 0.010(5) -0.006(5) -0.016(5) C14 0.024(6) 0.025(5) 0.043(6) 0.010(5) -0.015(5) -0.006(5) C15 0.033(7) 0.027(6) 0.048(6) -0.003(5) -0.017(6) -0.010(5) C16 0.039(7) 0.041(6) 0.025(5) -0.004(5) -0.014(5) -0.001(5) C17 0.026(6) 0.035(6) 0.064(7) 0.017(5) -0.016(5) -0.010(5) C18 0.017(6) 0.037(6) 0.056(7) -0.001(5) -0.014(5) -0.011(5) C19 0.039(7) 0.039(6) 0.038(6) -0.001(5) -0.004(5) -0.011(5) C20 0.041(7) 0.027(5) 0.039(6) 0.000(5) -0.010(5) -0.015(5) C21 0.031(6) 0.025(6) 0.036(6) 0.000(5) -0.006(5) -0.009(5) C22 0.047(8) 0.054(7) 0.039(6) 0.007(6) -0.008(6) 0.001(6) C23 0.038(7) 0.040(6) 0.063(7) -0.006(6) -0.008(6) 0.002(5) N24 0.042(5) 0.030(5) 0.027(5) 0.003(4) -0.004(4) -0.010(4) C25 0.068(9) 0.043(7) 0.032(6) -0.010(5) -0.010(6) 0.002(6) C26 0.074(9) 0.052(8) 0.033(7) -0.003(6) -0.021(6) -0.006(6) N27 0.034(5) 0.041(5) 0.036(5) 0.004(4) -0.009(4) -0.002(4) C28 0.033(7) 0.059(8) 0.038(7) 0.008(6) -0.006(5) -0.005(6) C29 0.072(9) 0.055(8) 0.072(8) 0.022(7) -0.026(7) -0.005(7) O30 0.173(10) 0.067(6) 0.106(7) 0.047(5) -0.037(7) -0.014(6) C31 0.104(11) 0.092(10) 0.037(7) 0.012(7) -0.037(7) 0.001(8) C32 0.177(16) 0.094(11) 0.049(8) -0.012(8) -0.055(9) 0.028(11) C33 0.119(12) 0.077(9) 0.066(8) -0.018(7) -0.050(8) 0.009(8) P1 0.042(2) 0.0447(18) 0.0508(18) 0.0011(15) -0.0211(15) -0.0058(15) F1 0.061(4) 0.059(4) 0.075(4) -0.020(3) -0.024(3) 0.004(3) F2 0.109(6) 0.089(5) 0.074(4) -0.038(4) -0.043(4) -0.001(4) F3 0.043(4) 0.065(4) 0.111(5) 0.006(3) -0.045(4) -0.013(3) F4 0.062(4) 0.059(4) 0.064(4) 0.022(3) -0.022(3) -0.018(3) F5 0.039(4) 0.084(4) 0.073(4) -0.002(3) -0.023(3) -0.003(3) F6 0.094(5) 0.088(5) 0.070(4) 0.036(3) -0.036(4) -0.045(4) N100 0.165(16) 0.152(17) 0.131(14) -0.050(10) -0.028(12) -0.006(13) C101 0.079(13) 0.127(19) 0.15(2) -0.046(13) -0.013(14) -0.047(14) C102 0.147(17) 0.103(13) 0.168(16) -0.012(11) -0.057(14) -0.048(12) _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 Cu1 N4 2.018(7) 2_864 ? Cu1 N27 2.022(7) . ? Cu1 N24 2.025(7) . ? Cu1 N10 2.032(7) 2_864 ? C2 O1A 1.31(2) . ? C2 O1 1.412(12) . ? C2 C3 1.466(12) . ? C3 N4 1.332(11) . ? C3 C8 1.401(12) . ? N4 C5 1.338(10) . ? N4 Cu1 2.018(7) 2_864 ? C5 C6 1.381(11) . ? C5 C9 1.462(11) . ? C6 C7 1.404(13) . ? C7 C8 1.358(12) . ? C9 N10 1.285(9) . ? N10 C11 1.440(10) . ? N10 Cu1 2.032(7) 2_864 ? C11 C12 1.388(10) . ? C11 C16 1.419(11) . ? C12 C13 1.384(11) . ? C13 C14 1.409(11) . ? C14 C15 1.369(11) . ? C14 C17 1.514(9) . ? C15 C16 1.404(11) . ? C17 C18 1.5409 . ? C18 C23 1.379(10) . ? C18 C19 1.3901 . ? C19 C20 1.404(9) . ? C20 C21 1.388(10) . ? C21 C22 1.362(12) . ? C21 N24 1.432(10) . ? C22 C23 1.393(11) . ? N24 C25 1.281(10) . ? C25 C26 1.421(12) . ? C26 N27 1.328(10) . ? C26 C33 1.381(11) . ? N27 C28 1.358(10) . ? C28 C31 1.388(13) . ? C28 C29 1.480(13) . ? C29 O30 1.347(10) . ? C31 C32 1.316(13) . ? C32 C33 1.3889 . ? P1 F2 1.564(6) . ? P1 F6 1.580(5) . ? P1 F4 1.594(5) . ? P1 F3 1.599(6) . ? P1 F5 1.607(6) . ? P1 F1 1.614(5) . ? N100 C101 1.155(19) . ? C101 C102 1.41(2) . ? N200 C201 1.11(2) . ? C201 C202 1.35(2) . ? N300 C301 0.89(6) . ? C301 C302 1.30(7) . ? N400 C401 0.72(5) . ? C401 C402 1.80(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 N4 Cu1 N27 123.1(3) 2_864 . ? N4 Cu1 N24 131.1(3) 2_864 . ? N27 Cu1 N24 81.1(3) . . ? N4 Cu1 N10 82.1(3) 2_864 2_864 ? N27 Cu1 N10 125.9(3) . 2_864 ? N24 Cu1 N10 119.9(3) . 2_864 ? O1A C2 O1 72.6(12) . . ? O1A C2 C3 109.2(13) . . ? O1 C2 C3 116.8(9) . . ? N4 C3 C8 121.4(9) . . ? N4 C3 C2 115.7(9) . . ? C8 C3 C2 122.9(10) . . ? C3 N4 C5 118.7(8) . . ? C3 N4 Cu1 129.9(7) . 2_864 ? C5 N4 Cu1 111.4(6) . 2_864 ? N4 C5 C6 123.8(9) . . ? N4 C5 C9 116.5(8) . . ? C6 C5 C9 119.7(10) . . ? C5 C6 C7 116.6(10) . . ? C8 C7 C6 120.1(10) . . ? C7 C8 C3 119.2(9) . . ? N10 C9 C5 117.9(8) . . ? C9 N10 C11 119.9(8) . . ? C9 N10 Cu1 112.2(6) . 2_864 ? C11 N10 Cu1 127.8(6) . 2_864 ? C12 C11 C16 119.5(8) . . ? C12 C11 N10 125.0(8) . . ? C16 C11 N10 115.4(8) . . ? C13 C12 C11 118.8(8) . . ? C12 C13 C14 122.3(9) . . ? C15 C14 C13 118.9(8) . . ? C15 C14 C17 120.9(8) . . ? C13 C14 C17 120.1(8) . . ? C14 C15 C16 120.1(8) . . ? C15 C16 C11 120.3(8) . . ? C14 C17 C18 111.1(3) . . ? C23 C18 C19 119.1(4) . . ? C23 C18 C17 122.1(4) . . ? C19 C18 C17 118.7 . . ? C18 C19 C20 120.0(5) . . ? C21 C20 C19 119.9(8) . . ? C22 C21 C20 119.7(8) . . ? C22 C21 N24 122.7(8) . . ? C20 C21 N24 117.6(8) . . ? C21 C22 C23 120.8(9) . . ? C18 C23 C22 120.5(9) . . ? C25 N24 C21 119.0(7) . . ? C25 N24 Cu1 112.2(6) . . ? C21 N24 Cu1 128.8(6) . . ? N24 C25 C26 118.6(9) . . ? N27 C26 C33 120.8(9) . . ? N27 C26 C25 116.7(8) . . ? C33 C26 C25 122.5(10) . . ? C26 N27 C28 119.3(8) . . ? C26 N27 Cu1 111.5(6) . . ? C28 N27 Cu1 129.2(7) . . ? N27 C28 C31 120.3(10) . . ? N27 C28 C29 115.8(9) . . ? C31 C28 C29 123.9(10) . . ? O30 C29 C28 113.3(9) . . ? C32 C31 C28 121.0(10) . . ? C31 C32 C33 118.9(6) . . ? C26 C33 C32 119.7(6) . . ? F2 P1 F6 91.8(3) . . ? F2 P1 F4 89.8(3) . . ? F6 P1 F4 178.4(3) . . ? F2 P1 F3 89.7(3) . . ? F6 P1 F3 89.8(3) . . ? F4 P1 F3 90.2(3) . . ? F2 P1 F5 91.3(3) . . ? F6 P1 F5 90.2(3) . . ? F4 P1 F5 89.7(3) . . ? F3 P1 F5 179.0(4) . . ? F2 P1 F1 178.8(4) . . ? F6 P1 F1 89.1(3) . . ? F4 P1 F1 89.3(3) . . ? F3 P1 F1 89.5(3) . . ? F5 P1 F1 89.5(3) . . ? N100 C101 C102 175(2) . . ? N200 C201 C202 174(2) . . ? N300 C301 C302 147(7) . . ? N400 C401 C402 147(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C9 H9A F4 0.95 2.74 3.323(10) 120.1 . O1A H1A N400 0.84 2.15 2.58(4) 111.2 . O30 H30 O1 0.84 2.22 2.676(11) 114.3 1_664 O30 H30 O1A 0.84 1.98 2.68(2) 140.3 1_664 C7 H7A F3 0.95 2.52 3.291(11) 138.2 1_455 C7 H7A F4 0.95 2.60 3.436(12) 146.9 1_455 C32 H32D F6 0.95 2.54 3.274(11) 134.4 1_564 C31 H31A F2 0.95 2.72 3.544(12) 145.6 1_564 C25 H25A N200 0.95 2.83 3.62(2) 141.1 1_654 C33 H33A N200 0.96 2.49 3.39(2) 154.8 1_654 C9 H9A F1 0.95 2.70 3.160(9) 110.5 2_854 C6 H6A F4 0.95 2.60 3.390(11) 140.2 2_854 C12 H12A F5 0.95 2.56 3.383(11) 145.6 2_854 C29 H29A F2 0.99 2.65 3.446(13) 137.8 2_864 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.504 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.085 data_al3 _database_code_CSD 211776 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H94 Cu2 F12 N10 O6 P2' _chemical_formula_weight 1660.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3955(14) _cell_length_b 15.0429(18) _cell_length_c 41.729(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.315(3) _cell_angle_gamma 90.00 _cell_volume 7717.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7308 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 35334 _diffrn_reflns_av_R_equivalents 0.1508 _diffrn_reflns_av_sigmaI/netI 0.1878 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.00 _reflns_number_total 12082 _reflns_number_gt 5951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00122(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12082 _refine_ls_number_parameters 1009 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1792 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 Cu1 Cu 0.06269(6) 1.17777(6) 0.391607(18) 0.0261(2) Uani 1 1 d . . . Cu2 Cu -0.02987(6) 1.24759(6) 0.114466(17) 0.0242(2) Uani 1 1 d . . . C103 C 0.2623(5) 1.2001(4) 0.44690(14) 0.0211(16) Uani 1 1 d . . . O101 O 0.2091(4) 1.0879(3) 0.48310(11) 0.0412(14) Uani 1 1 d . . . H10A H 0.260(5) 1.070(5) 0.5002(16) 0.062 Uiso 1 1 d . . . C102 C 0.2539(5) 1.1025(4) 0.45429(15) 0.0289(18) Uani 1 1 d . . . H10B H 0.2079 1.0730 0.4362 0.035 Uiso 1 1 calc R . . H10C H 0.3272 1.0755 0.4561 0.035 Uiso 1 1 calc R . . N104 N 0.1952(4) 1.2336(4) 0.42165(11) 0.0203(13) Uani 1 1 d . . . C105 C 0.2049(5) 1.3204(5) 0.41495(14) 0.0220(16) Uani 1 1 d . . . C106 C 0.2786(5) 1.3763(5) 0.43207(15) 0.0308(18) Uani 1 1 d . . . H10D H 0.2836 1.4371 0.4262 0.037 Uiso 1 1 calc R . . C107 C 0.3461(5) 1.3413(5) 0.45837(15) 0.0322(19) Uani 1 1 d . . . H10E H 0.3972 1.3781 0.4710 0.039 Uiso 1 1 calc R . . C108 C 0.3374(5) 1.2530(5) 0.46561(15) 0.0338(18) Uani 1 1 d . . . H10F H 0.3828 1.2281 0.4834 0.041 Uiso 1 1 calc R . . C109 C 0.1295(5) 1.3532(4) 0.38747(14) 0.0253(17) Uani 1 1 d . . . H10G H 0.1363 1.4120 0.3797 0.030 Uiso 1 1 calc R . . N110 N 0.0551(4) 1.3023(3) 0.37416(11) 0.0200(13) Uani 1 1 d . . . C111 C -0.0108(5) 1.3366(4) 0.34539(14) 0.0217(16) Uani 1 1 d . . . C112 C 0.0359(5) 1.3376(4) 0.31638(15) 0.0233(17) Uani 1 1 d . . . C113 C 0.1491(5) 1.3041(5) 0.31449(14) 0.0314(19) Uani 1 1 d . . . H11A H 0.1680 1.2609 0.3322 0.038 Uiso 1 1 calc R . . H11B H 0.2001 1.3548 0.3183 0.038 Uiso 1 1 calc R . . C114 C 0.1666(5) 1.2601(4) 0.28280(13) 0.0280(17) Uani 1 1 d . . . H11C H 0.2399 1.2346 0.2847 0.042 Uiso 1 1 calc R . . H11D H 0.1585 1.3045 0.2655 0.042 Uiso 1 1 calc R . . H11E H 0.1128 1.2128 0.2778 0.042 Uiso 1 1 calc R . . C115 C -0.0297(5) 1.3707(4) 0.28882(14) 0.0237(17) Uani 1 1 d . . . H11F H -0.0005 1.3735 0.2689 0.028 Uiso 1 1 calc R . . C116 C -0.1349(5) 1.3989(4) 0.28998(15) 0.0224(16) Uani 1 1 d . . . C117 C -0.1771(5) 1.3944(4) 0.31893(14) 0.0248(17) Uani 1 1 d . . . H11G H -0.2497 1.4137 0.3197 0.030 Uiso 1 1 calc R . . C118 C -0.1174(5) 1.3626(4) 0.34697(14) 0.0189(16) Uani 1 1 d . . . C119 C -0.1665(5) 1.3604(5) 0.37834(14) 0.0323(19) Uani 1 1 d . . . H11H H -0.1374 1.3085 0.3912 0.039 Uiso 1 1 calc R . . H11I H -0.2463 1.3529 0.3735 0.039 Uiso 1 1 calc R . . C120 C -0.1423(6) 1.4448(6) 0.39819(17) 0.064(3) Uani 1 1 d . . . H12A H -0.1746 1.4401 0.4184 0.096 Uiso 1 1 calc R . . H12B H -0.1733 1.4962 0.3858 0.096 Uiso 1 1 calc R . . H12C H -0.0634 1.4524 0.4031 0.096 Uiso 1 1 calc R . . C121 C -0.2037(5) 1.4375(5) 0.25981(13) 0.0294(18) Uani 1 1 d . . . H12D H -0.2815 1.4327 0.2627 0.035 Uiso 1 1 calc R . . H12E H -0.1864 1.5015 0.2583 0.035 Uiso 1 1 calc R . . C122 C -0.1869(5) 1.3928(5) 0.22793(15) 0.0261(17) Uani 1 1 d . . . C123 C -0.1542(5) 1.4450(4) 0.20308(15) 0.0236(17) Uani 1 1 d . . . H12F H -0.1383 1.5063 0.2066 0.028 Uiso 1 1 calc R . . C124 C -0.1451(5) 1.4061(4) 0.17300(14) 0.0200(16) Uani 1 1 d . . . C125 C -0.1133(5) 1.4652(4) 0.14613(14) 0.0265(17) Uani 1 1 d . . . H12G H -0.0653 1.5132 0.1559 0.032 Uiso 1 1 calc R . . H12H H -0.0712 1.4295 0.1321 0.032 Uiso 1 1 calc R . . C126 C -0.2095(6) 1.5067(5) 0.12542(16) 0.050(2) Uani 1 1 d . . . H12I H -0.1833 1.5457 0.1093 0.074 Uiso 1 1 calc R . . H12J H -0.2524 1.5415 0.1391 0.074 Uiso 1 1 calc R . . H12K H -0.2550 1.4597 0.1145 0.074 Uiso 1 1 calc R . . C127 C -0.1695(5) 1.3174(5) 0.16854(14) 0.0219(16) Uani 1 1 d . . . C128 C -0.1970(5) 1.2626(5) 0.19345(15) 0.0230(16) Uani 1 1 d . . . C129 C -0.2061(5) 1.1641(4) 0.19171(14) 0.0279(18) Uani 1 1 d . . . H12L H -0.2250 1.1461 0.1689 0.034 Uiso 1 1 calc R . . H12N H -0.2657 1.1446 0.2038 0.034 Uiso 1 1 calc R . . C130 C -0.1006(5) 1.1174(5) 0.20569(17) 0.048(2) Uani 1 1 d . . . H13A H -0.1113 1.0529 0.2047 0.072 Uiso 1 1 calc R . . H13B H -0.0808 1.1358 0.2282 0.072 Uiso 1 1 calc R . . H13D H -0.0422 1.1338 0.1931 0.072 Uiso 1 1 calc R . . C131 C -0.2064(4) 1.3047(5) 0.22293(15) 0.0223(16) Uani 1 1 d . . . H13E H -0.2272 1.2701 0.2402 0.027 Uiso 1 1 calc R . . N132 N -0.1612(4) 1.2777(3) 0.13697(11) 0.0220(14) Uani 1 1 d . . . C133 C -0.2502(5) 1.2493(5) 0.12107(14) 0.0235(16) Uani 1 1 d . . . H13F H -0.3175 1.2596 0.1291 0.028 Uiso 1 1 calc R . . C134 C -0.2481(5) 1.2012(4) 0.09090(14) 0.0217(16) Uani 1 1 d . . . N135 N -0.1474(4) 1.1845(4) 0.08274(11) 0.0205(13) Uani 1 1 d . . . C136 C -0.1406(5) 1.1387(4) 0.05575(15) 0.0205(16) Uani 1 1 d . . . C137 C -0.2312(5) 1.1061(5) 0.03629(15) 0.0328(19) Uani 1 1 d . . . H13G H -0.2231 1.0733 0.0173 0.039 Uiso 1 1 calc R . . C138 C -0.3330(6) 1.1221(5) 0.04497(16) 0.037(2) Uani 1 1 d . . . H13H H -0.3961 1.0990 0.0324 0.044 Uiso 1 1 calc R . . C139 C -0.3416(5) 1.1726(5) 0.07227(15) 0.0314(18) Uani 1 1 d . . . H13I H -0.4110 1.1873 0.0781 0.038 Uiso 1 1 calc R . . C140 C -0.0260(5) 1.1290(5) 0.04683(15) 0.0283(18) Uani 1 1 d . . . H14A H -0.0058 1.1835 0.0357 0.034 Uiso 1 1 calc R . . H14B H 0.0260 1.1215 0.0667 0.034 Uiso 1 1 calc R . . O141 O -0.0200(4) 1.0557(4) 0.02669(11) 0.0544(16) Uani 1 1 d . . . H14C H 0.0436 1.0510 0.0219 0.082 Uiso 1 1 calc R . . O201 O -0.1180(4) 1.1942(4) 0.48533(12) 0.0692(18) Uani 1 1 d . . . H20A H -0.1206 1.2466 0.4921 0.104 Uiso 1 1 calc R . . C202 C -0.0591(6) 1.1921(5) 0.45899(16) 0.047(2) Uani 1 1 d . . . H20B H 0.0155 1.2146 0.4656 0.056 Uiso 1 1 calc R . . H20C H -0.0944 1.2311 0.4416 0.056 Uiso 1 1 calc R . . C203 C -0.0540(5) 1.0988(5) 0.44663(16) 0.0277(17) Uani 1 1 d . . . N204 N -0.0149(4) 1.0886(4) 0.41825(12) 0.0234(14) Uani 1 1 d . . . C205 C -0.0055(5) 1.0044(5) 0.40737(14) 0.0198(16) Uani 1 1 d . . . C206 C -0.0354(5) 0.9306(5) 0.42349(15) 0.0291(18) Uani 1 1 d . . . H20D H -0.0283 0.8727 0.4149 0.035 Uiso 1 1 calc R . . C207 C -0.0760(5) 0.9426(5) 0.45261(15) 0.0313(19) Uani 1 1 d . . . H20E H -0.0968 0.8928 0.4644 0.038 Uiso 1 1 calc R . . C208 C -0.0858(5) 1.0270(5) 0.46413(16) 0.0346(19) Uani 1 1 d . . . H20F H -0.1141 1.0364 0.4840 0.042 Uiso 1 1 calc R . . C209 C 0.0388(5) 0.9978(5) 0.37629(13) 0.0221(17) Uani 1 1 d . . . H20G H 0.0396 0.9420 0.3657 0.027 Uiso 1 1 calc R . . N210 N 0.0765(4) 1.0669(4) 0.36349(11) 0.0214(13) Uani 1 1 d . . . C211 C 0.1144(5) 1.0529(4) 0.33254(14) 0.0208(16) Uani 1 1 d . . . C212 C 0.0408(5) 1.0251(4) 0.30594(14) 0.0208(16) Uani 1 1 d . . . C213 C -0.0815(5) 1.0259(5) 0.30636(14) 0.0289(18) Uani 1 1 d . . . H21A H -0.0991 0.9930 0.3256 0.035 Uiso 1 1 calc R . . H21B H -0.1171 0.9949 0.2869 0.035 Uiso 1 1 calc R . . C214 C -0.1266(5) 1.1200(5) 0.30713(16) 0.041(2) Uani 1 1 d . . . H21C H -0.2061 1.1176 0.3055 0.062 Uiso 1 1 calc R . . H21D H -0.1053 1.1540 0.2889 0.062 Uiso 1 1 calc R . . H21E H -0.0974 1.1489 0.3274 0.062 Uiso 1 1 calc R . . C215 C 0.0830(5) 1.0043(4) 0.27754(14) 0.0268(18) Uani 1 1 d . . . H21F H 0.0352 0.9841 0.2594 0.032 Uiso 1 1 calc R . . C216 C 0.1946(5) 1.0124(4) 0.27499(13) 0.0172(16) Uani 1 1 d . . . C217 C 0.2612(5) 1.0458(4) 0.30096(15) 0.0227(17) Uani 1 1 d . . . H21G H 0.3357 1.0555 0.2989 0.027 Uiso 1 1 calc R . . C218 C 0.2238(5) 1.0662(4) 0.33020(14) 0.0183(16) Uani 1 1 d . . . C219 C 0.3041(4) 1.0957(4) 0.35839(14) 0.0204(16) Uani 1 1 d . . . H21H H 0.2689 1.1397 0.3713 0.025 Uiso 1 1 calc R . . H21I H 0.3665 1.1251 0.3502 0.025 Uiso 1 1 calc R . . C220 C 0.3455(5) 1.0186(5) 0.37999(14) 0.0333(19) Uani 1 1 d . . . H22A H 0.4037 1.0394 0.3964 0.050 Uiso 1 1 calc R . . H22B H 0.3738 0.9720 0.3669 0.050 Uiso 1 1 calc R . . H22C H 0.2858 0.9945 0.3906 0.050 Uiso 1 1 calc R . . C221 C 0.2382(5) 0.9816(5) 0.24418(14) 0.0300(18) Uani 1 1 d . . . H22D H 0.3186 0.9798 0.2482 0.036 Uiso 1 1 calc R . . H22E H 0.2123 0.9203 0.2392 0.036 Uiso 1 1 calc R . . C222 C 0.2043(5) 1.0402(4) 0.21492(14) 0.0169(15) Uani 1 1 d . . . C223 C 0.2260(5) 1.1314(5) 0.21648(15) 0.0221(17) Uani 1 1 d . . . H22F H 0.2592 1.1566 0.2362 0.027 Uiso 1 1 calc R . . C224 C 0.1998(4) 1.1855(4) 0.18971(14) 0.0181(15) Uani 1 1 d . . . C225 C 0.2163(5) 1.2848(4) 0.19338(14) 0.0246(17) Uani 1 1 d . . . H22G H 0.2534 1.3074 0.1753 0.030 Uiso 1 1 calc R . . H22H H 0.2636 1.2973 0.2138 0.030 Uiso 1 1 calc R . . C226 C 0.1067(5) 1.3335(4) 0.19347(14) 0.0264(17) Uani 1 1 d . . . H22I H 0.1202 1.3960 0.1993 0.040 Uiso 1 1 calc R . . H22J H 0.0653 1.3054 0.2092 0.040 Uiso 1 1 calc R . . H22K H 0.0651 1.3301 0.1719 0.040 Uiso 1 1 calc R . . C227 C 0.1507(4) 1.1467(4) 0.16068(14) 0.0158(15) Uani 1 1 d . . . C228 C 0.1279(5) 1.0563(4) 0.15900(14) 0.0190(16) Uani 1 1 d . . . C229 C 0.0724(5) 1.0121(5) 0.12848(14) 0.0306(18) Uani 1 1 d . . . H22L H 0.0861 1.0477 0.1094 0.037 Uiso 1 1 calc R . . H22M H 0.1040 0.9523 0.1264 0.037 Uiso 1 1 calc R . . C230 C -0.0493(5) 1.0036(5) 0.12900(16) 0.049(2) Uani 1 1 d . . . H23A H -0.0833 0.9808 0.1081 0.073 Uiso 1 1 calc R . . H23C H -0.0799 1.0621 0.1330 0.073 Uiso 1 1 calc R . . H23D H -0.0633 0.9625 0.1462 0.073 Uiso 1 1 calc R . . C231 C 0.1558(5) 1.0039(4) 0.18638(15) 0.0243(17) Uani 1 1 d . . . H23E H 0.1411 0.9420 0.1853 0.029 Uiso 1 1 calc R . . N232 N 0.1194(4) 1.2023(3) 0.13300(11) 0.0186(13) Uani 1 1 d . . . C233 C 0.1962(5) 1.2392(4) 0.11941(13) 0.0222(16) Uani 1 1 d . . . H23F H 0.2702 1.2276 0.1273 0.027 Uiso 1 1 calc R . . C234 C 0.1695(5) 1.2978(4) 0.09219(14) 0.0199(16) Uani 1 1 d . . . N235 N 0.0616(4) 1.3195(3) 0.08540(11) 0.0199(13) Uani 1 1 d . . . C236 C 0.0309(5) 1.3707(4) 0.05901(14) 0.0218(16) Uani 1 1 d . . . C237 C 0.1063(6) 1.3997(5) 0.03954(15) 0.0312(19) Uani 1 1 d . . . H23G H 0.0829 1.4345 0.0209 0.037 Uiso 1 1 calc R . . C238 C 0.2150(6) 1.3789(5) 0.04680(16) 0.0359(19) Uani 1 1 d . . . H23H H 0.2664 1.3992 0.0334 0.043 Uiso 1 1 calc R . . C239 C 0.2477(5) 1.3283(4) 0.07380(15) 0.0276(17) Uani 1 1 d . . . H23I H 0.3223 1.3146 0.0797 0.033 Uiso 1 1 calc R . . C240 C -0.0884(5) 1.3904(5) 0.05312(14) 0.0284(18) Uani 1 1 d . . . H24A H -0.1287 1.3342 0.0485 0.034 Uiso 1 1 calc R . . H24B H -0.1116 1.4161 0.0730 0.034 Uiso 1 1 calc R . . O241 O -0.1159(4) 1.4504(3) 0.02709(10) 0.0370(14) Uani 1 1 d . . . H24G H -0.105(5) 1.510(5) 0.0335(16) 0.055 Uiso 1 1 d . . . O11 O 0.0189(4) 0.7757(4) 0.36420(14) 0.0600(17) Uani 1 1 d . . . C12 C 0.0059(6) 0.7494(7) 0.3354(2) 0.056(2) Uani 1 1 d . . . H12M H -0.0120 0.7937 0.3194 0.068 Uiso 1 1 calc R . . C13 C 0.0407(7) 0.5976(6) 0.3471(2) 0.076(3) Uani 1 1 d . . . H13C H 0.0433 0.6188 0.3694 0.114 Uiso 1 1 calc R . . H13J H 0.1117 0.5732 0.3438 0.114 Uiso 1 1 calc R . . H13K H -0.0148 0.5512 0.3430 0.114 Uiso 1 1 calc R . . N13 N 0.0140(4) 0.6702(5) 0.32518(15) 0.0443(17) Uani 1 1 d . . . C14 C -0.0039(6) 0.6452(7) 0.2912(2) 0.100(4) Uani 1 1 d . . . H14D H -0.0225 0.6981 0.2780 0.150 Uiso 1 1 calc R . . H14E H -0.0636 0.6022 0.2877 0.150 Uiso 1 1 calc R . . H14F H 0.0625 0.6183 0.2850 0.150 Uiso 1 1 calc R . . O21 O -0.0620(4) 0.6052(4) 0.05302(12) 0.0583(16) Uani 1 1 d . . . C22 C -0.1010(6) 0.6800(6) 0.04688(18) 0.042(2) Uani 1 1 d . . . H22N H -0.1437 0.6885 0.0265 0.050 Uiso 1 1 calc R . . N23 N -0.0874(4) 0.7482(5) 0.06650(13) 0.0385(15) Uani 1 1 d . . . C23 C -0.0246(6) 0.7399(6) 0.09840(15) 0.060(2) Uani 1 1 d . . . H23B H 0.0165 0.6841 0.0996 0.090 Uiso 1 1 calc R . . H23J H -0.0740 0.7400 0.1149 0.090 Uiso 1 1 calc R . . H23K H 0.0260 0.7900 0.1021 0.090 Uiso 1 1 calc R . . C24 C -0.1347(6) 0.8349(6) 0.05672(17) 0.061(3) Uani 1 1 d . . . H24D H -0.1728 0.8308 0.0347 0.092 Uiso 1 1 calc R . . H24E H -0.0767 0.8793 0.0574 0.092 Uiso 1 1 calc R . . H24F H -0.1863 0.8523 0.0715 0.092 Uiso 1 1 calc R . . P10 P 0.31092(16) 0.10590(14) 0.03551(5) 0.0370(5) Uani 1 1 d . . . F11 F 0.3900(3) 0.0273(3) 0.04674(10) 0.0697(14) Uani 1 1 d . . . F12 F 0.2291(3) 0.1848(3) 0.02377(9) 0.0471(11) Uani 1 1 d . . . F13 F 0.2657(3) 0.1056(3) 0.06954(9) 0.0563(13) Uani 1 1 d . . . F14 F 0.3545(4) 0.1069(3) 0.00084(10) 0.0731(15) Uani 1 1 d . . . F15 F 0.4001(3) 0.1780(3) 0.04867(11) 0.0725(14) Uani 1 1 d . . . F16 F 0.2173(3) 0.0365(3) 0.02215(9) 0.0484(12) Uani 1 1 d . . . P20 P -0.47187(15) 1.25702(16) 0.29945(5) 0.0414(6) Uani 1 1 d . . . F21 F -0.5637(3) 1.2745(3) 0.32223(10) 0.0650(15) Uani 1 1 d . A . F22 F -0.3802(3) 1.2412(3) 0.27689(10) 0.0722(15) Uani 1 1 d . A . F23 F -0.5628(5) 1.2703(7) 0.26909(13) 0.089(3) Uani 0.875(11) 1 d P A 1 F24 F -0.3797(4) 1.2522(6) 0.32923(12) 0.083(3) Uani 0.875(11) 1 d P A 1 F25 F -0.4504(5) 1.3628(4) 0.2979(2) 0.089(3) Uani 0.875(11) 1 d P A 1 F26 F -0.4941(6) 1.1557(4) 0.3001(3) 0.112(4) Uani 0.875(11) 1 d P A 1 F23A F -0.548(3) 1.189(3) 0.2797(8) 0.032(11) Uiso 0.125(11) 1 d P A 2 F24A F -0.422(3) 1.323(3) 0.3226(10) 0.052(14) Uiso 0.125(11) 1 d P A 2 F25A F -0.508(4) 1.313(3) 0.2743(11) 0.059(15) Uiso 0.125(11) 1 d P A 2 F26A F -0.426(3) 1.184(2) 0.3269(7) 0.026(11) Uiso 0.125(11) 1 d P A 2 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 Cu1 0.0333(5) 0.0226(5) 0.0220(5) 0.0004(4) 0.0015(4) -0.0036(4) Cu2 0.0186(5) 0.0324(6) 0.0218(5) -0.0012(4) 0.0033(3) -0.0023(4) C103 0.028(4) 0.026(5) 0.011(4) -0.001(3) 0.008(3) -0.002(3) O101 0.042(4) 0.047(4) 0.036(3) 0.021(3) 0.010(3) 0.005(3) C102 0.032(5) 0.029(5) 0.023(4) 0.003(4) -0.011(3) -0.003(3) N104 0.026(3) 0.020(4) 0.016(3) 0.002(3) 0.001(2) -0.001(3) C105 0.024(4) 0.028(5) 0.015(4) -0.001(4) 0.006(3) -0.004(4) C106 0.039(5) 0.028(5) 0.026(4) -0.004(4) 0.008(4) 0.002(4) C107 0.038(5) 0.033(5) 0.023(4) -0.007(4) -0.003(3) -0.005(4) C108 0.038(5) 0.043(5) 0.020(4) -0.001(4) 0.001(3) -0.002(4) C109 0.038(5) 0.012(4) 0.026(4) 0.006(3) 0.006(3) 0.003(3) N110 0.024(3) 0.019(4) 0.018(3) 0.004(3) 0.003(3) 0.000(3) C111 0.035(5) 0.010(4) 0.019(4) 0.001(3) -0.004(3) -0.008(3) C112 0.017(4) 0.030(5) 0.025(4) -0.002(3) 0.008(3) 0.000(3) C113 0.027(4) 0.039(5) 0.028(4) 0.002(4) 0.003(3) 0.009(4) C114 0.026(4) 0.036(5) 0.022(4) 0.003(4) 0.005(3) 0.004(3) C115 0.029(4) 0.027(5) 0.016(4) 0.000(3) 0.007(3) 0.009(3) C116 0.017(4) 0.026(5) 0.024(4) -0.005(3) 0.003(3) 0.008(3) C117 0.021(4) 0.029(5) 0.025(4) -0.002(3) 0.005(3) 0.005(3) C118 0.013(4) 0.019(4) 0.026(4) 0.000(3) 0.009(3) 0.001(3) C119 0.024(4) 0.049(6) 0.024(4) 0.004(4) 0.007(3) 0.000(4) C120 0.063(6) 0.093(8) 0.041(5) -0.029(5) 0.030(4) -0.021(5) C121 0.031(4) 0.040(5) 0.017(4) 0.001(3) 0.000(3) 0.018(3) C122 0.020(4) 0.037(5) 0.020(4) -0.003(4) -0.003(3) 0.010(3) C123 0.021(4) 0.020(4) 0.029(4) -0.002(4) 0.000(3) 0.004(3) C124 0.019(4) 0.022(5) 0.019(4) 0.001(3) 0.001(3) 0.004(3) C125 0.030(4) 0.033(5) 0.019(4) 0.001(3) 0.009(3) -0.005(3) C126 0.066(6) 0.048(6) 0.036(5) 0.020(4) 0.015(4) 0.023(5) C127 0.019(4) 0.033(5) 0.014(4) -0.005(4) 0.003(3) -0.003(3) C128 0.016(4) 0.025(5) 0.028(4) 0.001(4) 0.004(3) 0.001(3) C129 0.032(5) 0.032(5) 0.020(4) -0.001(3) 0.005(3) -0.008(4) C130 0.044(5) 0.037(6) 0.064(6) -0.006(4) 0.009(4) 0.004(4) C131 0.016(4) 0.029(5) 0.021(4) 0.006(4) 0.002(3) 0.000(3) N132 0.026(3) 0.024(4) 0.017(3) 0.000(3) 0.006(3) -0.006(3) C133 0.015(4) 0.031(4) 0.025(4) 0.001(4) 0.007(3) 0.000(4) C134 0.021(4) 0.019(4) 0.025(4) -0.006(3) 0.003(3) -0.007(3) N135 0.021(3) 0.025(4) 0.015(3) -0.005(3) 0.005(2) -0.003(3) C136 0.018(4) 0.021(4) 0.022(4) -0.001(3) 0.001(3) 0.002(3) C137 0.024(5) 0.051(6) 0.023(4) -0.014(4) 0.004(3) -0.007(4) C138 0.029(5) 0.046(6) 0.033(5) -0.012(4) -0.009(4) -0.015(4) C139 0.016(4) 0.047(5) 0.031(4) -0.006(4) 0.002(3) -0.004(4) C140 0.024(4) 0.031(5) 0.029(4) -0.017(4) 0.003(3) 0.006(3) O141 0.040(3) 0.066(4) 0.057(4) -0.027(3) 0.005(3) 0.006(3) O201 0.102(5) 0.051(4) 0.065(4) -0.017(3) 0.048(3) -0.001(3) C202 0.069(6) 0.045(6) 0.031(5) -0.008(4) 0.027(4) -0.005(4) C203 0.029(4) 0.023(5) 0.031(4) -0.006(4) 0.004(3) 0.001(3) N204 0.020(3) 0.026(4) 0.025(3) 0.003(3) 0.007(3) 0.005(3) C205 0.016(4) 0.029(5) 0.014(4) -0.001(3) -0.001(3) 0.000(3) C206 0.034(5) 0.030(5) 0.025(4) 0.004(4) 0.010(3) -0.011(3) C207 0.031(5) 0.034(5) 0.032(5) 0.010(4) 0.014(3) -0.003(4) C208 0.039(5) 0.040(6) 0.028(4) -0.002(4) 0.015(4) 0.000(4) C209 0.022(4) 0.031(5) 0.013(4) -0.005(3) 0.002(3) -0.003(3) N210 0.021(3) 0.023(4) 0.020(3) -0.002(3) 0.005(3) -0.003(3) C211 0.024(4) 0.020(4) 0.019(4) 0.000(3) 0.006(3) -0.001(3) C212 0.025(4) 0.020(4) 0.018(4) 0.008(3) 0.005(3) 0.001(3) C213 0.017(4) 0.045(5) 0.023(4) -0.007(4) -0.001(3) -0.006(3) C214 0.027(5) 0.040(6) 0.055(5) 0.012(4) -0.002(4) 0.008(4) C215 0.036(5) 0.030(5) 0.013(4) 0.003(3) -0.003(3) 0.000(4) C216 0.019(4) 0.024(4) 0.008(4) 0.009(3) 0.001(3) 0.007(3) C217 0.021(4) 0.021(4) 0.029(4) 0.014(3) 0.016(3) 0.006(3) C218 0.022(4) 0.012(4) 0.020(4) 0.002(3) 0.002(3) -0.003(3) C219 0.014(4) 0.019(4) 0.027(4) -0.001(3) 0.002(3) -0.004(3) C220 0.026(4) 0.039(5) 0.034(4) 0.005(4) -0.001(3) -0.005(4) C221 0.031(4) 0.032(5) 0.028(4) 0.006(4) 0.011(3) 0.012(4) C222 0.018(4) 0.022(4) 0.012(4) 0.000(3) 0.008(3) 0.010(3) C223 0.011(4) 0.037(5) 0.019(4) -0.004(4) 0.006(3) 0.004(3) C224 0.016(4) 0.017(4) 0.023(4) -0.003(4) 0.008(3) -0.005(3) C225 0.020(4) 0.036(5) 0.016(4) -0.004(3) -0.004(3) 0.000(3) C226 0.031(4) 0.024(5) 0.024(4) -0.004(3) 0.001(3) 0.002(3) C227 0.010(4) 0.026(5) 0.011(4) 0.008(3) 0.003(3) 0.004(3) C228 0.020(4) 0.020(5) 0.019(4) -0.002(3) 0.010(3) 0.002(3) C229 0.042(5) 0.030(5) 0.018(4) -0.003(3) -0.003(3) -0.006(4) C230 0.049(6) 0.044(6) 0.049(5) 0.002(4) -0.008(4) -0.009(4) C231 0.028(4) 0.018(4) 0.029(4) 0.003(4) 0.014(3) 0.008(3) N232 0.017(3) 0.022(4) 0.017(3) -0.006(3) 0.003(2) 0.001(3) C233 0.017(4) 0.029(5) 0.019(4) -0.004(3) -0.006(3) 0.005(3) C234 0.025(4) 0.012(4) 0.023(4) -0.003(3) 0.001(3) -0.007(3) N235 0.028(4) 0.018(3) 0.014(3) -0.005(3) 0.004(2) -0.002(3) C236 0.029(5) 0.022(4) 0.015(4) -0.005(3) 0.006(3) -0.002(3) C237 0.050(5) 0.027(5) 0.018(4) 0.005(3) 0.010(4) -0.006(4) C238 0.054(6) 0.022(5) 0.036(5) 0.000(4) 0.024(4) -0.004(4) C239 0.029(4) 0.023(5) 0.032(4) -0.005(4) 0.010(3) -0.008(3) C240 0.033(5) 0.034(5) 0.017(4) 0.002(4) -0.002(3) 0.004(4) O241 0.056(4) 0.030(3) 0.020(3) 0.005(3) -0.011(2) 0.001(3) O11 0.051(4) 0.056(5) 0.073(4) -0.029(4) 0.008(3) -0.004(3) C12 0.027(5) 0.046(7) 0.098(8) -0.007(6) 0.020(5) -0.004(5) C13 0.064(7) 0.053(7) 0.115(8) 0.001(7) 0.025(6) -0.009(5) N13 0.029(4) 0.058(6) 0.046(5) -0.004(4) 0.007(3) -0.001(4) C14 0.050(7) 0.192(14) 0.060(7) -0.045(7) 0.021(5) -0.011(6) O21 0.071(4) 0.040(4) 0.059(4) -0.007(3) -0.009(3) 0.008(3) C22 0.045(5) 0.047(6) 0.034(5) 0.000(5) 0.005(4) -0.005(5) N23 0.044(4) 0.046(5) 0.023(4) -0.006(4) -0.005(3) 0.002(4) C23 0.093(7) 0.059(7) 0.028(5) -0.012(5) 0.005(4) 0.012(5) C24 0.072(7) 0.062(7) 0.047(5) -0.005(5) -0.004(4) 0.026(5) P10 0.0352(13) 0.0324(14) 0.0440(14) -0.0001(11) 0.0066(10) 0.0008(10) F11 0.057(3) 0.057(4) 0.095(4) 0.013(3) 0.006(3) 0.023(3) F12 0.056(3) 0.036(3) 0.047(3) -0.002(2) -0.004(2) 0.010(2) F13 0.080(3) 0.061(3) 0.029(2) -0.006(2) 0.012(2) 0.003(3) F14 0.085(4) 0.075(4) 0.070(3) 0.007(3) 0.052(3) 0.007(3) F15 0.034(3) 0.055(4) 0.125(4) -0.016(3) -0.004(3) -0.015(2) F16 0.053(3) 0.037(3) 0.054(3) -0.015(2) 0.005(2) -0.015(2) P20 0.0299(13) 0.0471(16) 0.0479(14) -0.0008(13) 0.0074(11) -0.0043(12) F21 0.050(3) 0.087(4) 0.063(3) 0.003(3) 0.027(2) 0.010(3) F22 0.040(3) 0.113(5) 0.069(3) -0.014(3) 0.026(2) 0.007(3) F23 0.032(4) 0.173(10) 0.058(4) 0.001(4) -0.005(3) -0.003(5) F24 0.046(4) 0.141(9) 0.057(4) 0.019(4) -0.015(3) 0.007(5) F25 0.076(5) 0.044(4) 0.152(8) 0.012(5) 0.042(5) -0.014(3) F26 0.075(6) 0.028(4) 0.245(11) 0.000(5) 0.067(7) -0.004(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 Cu1 N110 2.007(5) . ? Cu1 N204 2.057(5) . ? Cu1 N210 2.058(5) . ? Cu1 N104 2.110(5) . ? Cu2 N232 2.030(5) . ? Cu2 N132 2.032(5) . ? Cu2 N235 2.069(5) . ? Cu2 N135 2.070(5) . ? C103 N104 1.354(7) . ? C103 C108 1.388(8) . ? C103 C102 1.506(9) . ? O101 C102 1.404(7) . ? N104 C105 1.344(8) . ? C105 C106 1.374(8) . ? C105 C109 1.469(8) . ? C106 C107 1.396(8) . ? C107 C108 1.369(9) . ? C109 N110 1.271(7) . ? N110 C111 1.458(7) . ? C111 C118 1.387(8) . ? C111 C112 1.407(8) . ? C112 C115 1.412(8) . ? C112 C113 1.502(8) . ? C113 C114 1.519(7) . ? C115 C116 1.378(8) . ? C116 C117 1.378(7) . ? C116 C121 1.541(8) . ? C117 C118 1.388(8) . ? C118 C119 1.513(7) . ? C119 C120 1.525(9) . ? C121 C122 1.529(8) . ? C122 C131 1.358(9) . ? C122 C123 1.402(8) . ? C123 C124 1.403(8) . ? C124 C127 1.375(8) . ? C124 C125 1.522(8) . ? C125 C126 1.515(8) . ? C127 C128 1.402(8) . ? C127 N132 1.462(7) . ? C128 C131 1.401(8) . ? C128 C129 1.488(9) . ? C129 C130 1.532(8) . ? N132 C133 1.286(7) . ? C133 C134 1.455(8) . ? C134 N135 1.358(7) . ? C134 C139 1.379(8) . ? N135 C136 1.332(7) . ? C136 C137 1.389(8) . ? C136 C140 1.521(8) . ? C137 C138 1.377(8) . ? C138 C139 1.384(8) . ? C140 O141 1.394(7) . ? O201 C202 1.395(7) . ? C202 C203 1.500(9) . ? C203 N204 1.344(7) . ? C203 C208 1.389(9) . ? N204 C205 1.355(8) . ? C205 C206 1.374(8) . ? C205 C209 1.475(7) . ? C206 C207 1.385(8) . ? C207 C208 1.368(9) . ? C209 N210 1.284(7) . ? N210 C211 1.445(7) . ? C211 C218 1.386(8) . ? C211 C212 1.408(8) . ? C212 C215 1.390(7) . ? C212 C213 1.518(7) . ? C213 C214 1.524(9) . ? C215 C216 1.407(7) . ? C216 C217 1.371(8) . ? C216 C221 1.528(7) . ? C217 C218 1.393(7) . ? C218 C219 1.508(8) . ? C219 C220 1.518(8) . ? C221 C222 1.521(8) . ? C222 C231 1.376(8) . ? C222 C223 1.398(8) . ? C223 C224 1.387(8) . ? C224 C227 1.411(8) . ? C224 C225 1.513(8) . ? C225 C226 1.544(8) . ? C227 C228 1.389(8) . ? C227 N232 1.439(7) . ? C228 C231 1.395(8) . ? C228 C229 1.521(8) . ? C229 C230 1.517(8) . ? N232 C233 1.293(7) . ? C233 C234 1.443(8) . ? C234 N235 1.371(7) . ? C234 C239 1.388(8) . ? N235 C236 1.358(7) . ? C236 C237 1.385(8) . ? C236 C240 1.497(8) . ? C237 C238 1.378(9) . ? C238 C239 1.377(8) . ? C240 O241 1.419(7) . ? O11 C12 1.256(9) . ? C12 N13 1.273(10) . ? C13 N13 1.436(9) . ? N13 C14 1.457(9) . ? O21 C22 1.238(9) . ? C22 N23 1.310(9) . ? N23 C23 1.459(8) . ? N23 C24 1.466(9) . ? P10 F11 1.569(4) . ? P10 F13 1.592(4) . ? P10 F15 1.596(4) . ? P10 F12 1.597(4) . ? P10 F14 1.607(4) . ? P10 F16 1.607(4) . ? P20 F25A 1.38(5) . ? P20 F24A 1.47(4) . ? P20 F26 1.549(6) . ? P20 F23A 1.56(3) . ? P20 F24 1.579(5) . ? P20 F22 1.583(4) . ? P20 F21 1.595(4) . ? P20 F23 1.597(6) . ? P20 F25 1.616(6) . ? P20 F26A 1.64(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N110 Cu1 N204 143.2(2) . . ? N110 Cu1 N210 123.5(2) . . ? N204 Cu1 N210 81.9(2) . . ? N110 Cu1 N104 80.8(2) . . ? N204 Cu1 N104 108.71(19) . . ? N210 Cu1 N104 123.10(19) . . ? N232 Cu2 N132 130.10(19) . . ? N232 Cu2 N235 81.8(2) . . ? N132 Cu2 N235 133.3(2) . . ? N232 Cu2 N135 128.5(2) . . ? N132 Cu2 N135 81.8(2) . . ? N235 Cu2 N135 104.99(18) . . ? N104 C103 C108 121.7(6) . . ? N104 C103 C102 118.1(6) . . ? C108 C103 C102 120.2(6) . . ? O101 C102 C103 111.9(5) . . ? C105 N104 C103 117.5(5) . . ? C105 N104 Cu1 110.3(4) . . ? C103 N104 Cu1 132.0(4) . . ? N104 C105 C106 123.9(6) . . ? N104 C105 C109 115.1(6) . . ? C106 C105 C109 121.0(7) . . ? C105 C106 C107 118.0(7) . . ? C108 C107 C106 118.9(7) . . ? C107 C108 C103 119.9(6) . . ? N110 C109 C105 119.5(6) . . ? C109 N110 C111 116.4(5) . . ? C109 N110 Cu1 114.0(4) . . ? C111 N110 Cu1 128.7(4) . . ? C118 C111 C112 122.5(6) . . ? C118 C111 N110 119.9(5) . . ? C112 C111 N110 117.6(6) . . ? C111 C112 C115 116.5(6) . . ? C111 C112 C113 122.1(6) . . ? C115 C112 C113 121.4(5) . . ? C112 C113 C114 115.5(5) . . ? C116 C115 C112 122.0(6) . . ? C117 C116 C115 118.8(6) . . ? C117 C116 C121 120.2(6) . . ? C115 C116 C121 121.0(5) . . ? C116 C117 C118 122.4(6) . . ? C111 C118 C117 117.8(5) . . ? C111 C118 C119 121.7(6) . . ? C117 C118 C119 120.4(6) . . ? C118 C119 C120 112.3(6) . . ? C122 C121 C116 115.0(5) . . ? C131 C122 C123 119.7(6) . . ? C131 C122 C121 121.5(6) . . ? C123 C122 C121 118.7(6) . . ? C122 C123 C124 119.4(6) . . ? C127 C124 C123 119.0(6) . . ? C127 C124 C125 122.7(6) . . ? C123 C124 C125 118.2(6) . . ? C126 C125 C124 113.7(5) . . ? C124 C127 C128 122.7(6) . . ? C124 C127 N132 118.6(5) . . ? C128 C127 N132 118.7(6) . . ? C131 C128 C127 116.1(6) . . ? C131 C128 C129 118.6(6) . . ? C127 C128 C129 125.0(6) . . ? C128 C129 C130 112.5(5) . . ? C122 C131 C128 122.9(6) . . ? C133 N132 C127 116.5(5) . . ? C133 N132 Cu2 111.9(4) . . ? C127 N132 Cu2 131.3(4) . . ? N132 C133 C134 120.2(5) . . ? N135 C134 C139 122.3(6) . . ? N135 C134 C133 115.3(5) . . ? C139 C134 C133 122.4(6) . . ? C136 N135 C134 117.8(5) . . ? C136 N135 Cu2 131.5(4) . . ? C134 N135 Cu2 110.4(4) . . ? N135 C136 C137 122.9(6) . . ? N135 C136 C140 114.7(5) . . ? C137 C136 C140 122.3(6) . . ? C138 C137 C136 118.9(6) . . ? C137 C138 C139 118.8(6) . . ? C134 C139 C138 119.2(6) . . ? O141 C140 C136 110.3(5) . . ? O201 C202 C203 109.9(6) . . ? N204 C203 C208 122.2(6) . . ? N204 C203 C202 116.4(6) . . ? C208 C203 C202 121.4(6) . . ? C203 N204 C205 117.2(6) . . ? C203 N204 Cu1 130.4(5) . . ? C205 N204 Cu1 111.2(4) . . ? N204 C205 C206 123.5(6) . . ? N204 C205 C209 114.6(6) . . ? C206 C205 C209 121.9(6) . . ? C205 C206 C207 118.3(7) . . ? C208 C207 C206 119.2(6) . . ? C207 C208 C203 119.6(6) . . ? N210 C209 C205 120.4(6) . . ? C209 N210 C211 115.5(5) . . ? C209 N210 Cu1 111.0(4) . . ? C211 N210 Cu1 133.4(4) . . ? C218 C211 C212 121.9(5) . . ? C218 C211 N210 118.3(5) . . ? C212 C211 N210 119.7(5) . . ? C215 C212 C211 117.5(6) . . ? C215 C212 C213 119.7(6) . . ? C211 C212 C213 122.4(5) . . ? C212 C213 C214 112.1(5) . . ? C212 C215 C216 121.7(6) . . ? C217 C216 C215 118.1(5) . . ? C217 C216 C221 122.3(6) . . ? C215 C216 C221 119.6(5) . . ? C216 C217 C218 122.6(6) . . ? C211 C218 C217 117.9(6) . . ? C211 C218 C219 122.8(5) . . ? C217 C218 C219 119.2(6) . . ? C218 C219 C220 112.2(5) . . ? C222 C221 C216 114.1(5) . . ? C231 C222 C223 119.3(6) . . ? C231 C222 C221 120.7(6) . . ? C223 C222 C221 119.9(6) . . ? C224 C223 C222 121.0(6) . . ? C223 C224 C227 118.7(6) . . ? C223 C224 C225 118.9(6) . . ? C227 C224 C225 122.2(6) . . ? C224 C225 C226 111.1(5) . . ? C228 C227 C224 120.7(6) . . ? C228 C227 N232 119.8(5) . . ? C224 C227 N232 119.5(6) . . ? C227 C228 C231 118.9(6) . . ? C227 C228 C229 122.5(6) . . ? C231 C228 C229 118.5(6) . . ? C230 C229 C228 111.7(5) . . ? C222 C231 C228 121.4(6) . . ? C233 N232 C227 117.6(5) . . ? C233 N232 Cu2 112.1(4) . . ? C227 N232 Cu2 129.8(4) . . ? N232 C233 C234 119.9(6) . . ? N235 C234 C239 122.5(6) . . ? N235 C234 C233 115.4(5) . . ? C239 C234 C233 122.1(6) . . ? C236 N235 C234 117.9(5) . . ? C236 N235 Cu2 130.8(4) . . ? C234 N235 Cu2 110.3(4) . . ? N235 C236 C237 120.9(6) . . ? N235 C236 C240 114.5(5) . . ? C237 C236 C240 124.6(6) . . ? C238 C237 C236 120.9(7) . . ? C239 C238 C237 118.9(6) . . ? C238 C239 C234 118.8(6) . . ? O241 C240 C236 112.8(5) . . ? O11 C12 N13 127.5(9) . . ? C12 N13 C13 121.3(8) . . ? C12 N13 C14 124.0(9) . . ? C13 N13 C14 114.6(8) . . ? O21 C22 N23 124.5(8) . . ? C22 N23 C23 121.0(7) . . ? C22 N23 C24 120.5(6) . . ? C23 N23 C24 118.5(6) . . ? F11 P10 F13 90.5(2) . . ? F11 P10 F15 91.7(3) . . ? F13 P10 F15 90.1(3) . . ? F11 P10 F12 179.1(3) . . ? F13 P10 F12 89.6(2) . . ? F15 P10 F12 89.2(3) . . ? F11 P10 F14 90.4(3) . . ? F13 P10 F14 179.0(3) . . ? F15 P10 F14 90.3(3) . . ? F12 P10 F14 89.4(2) . . ? F11 P10 F16 90.6(3) . . ? F13 P10 F16 89.2(2) . . ? F15 P10 F16 177.6(3) . . ? F12 P10 F16 88.5(2) . . ? F14 P10 F16 90.3(2) . . ? F25A P20 F24A 99(3) . . ? F25A P20 F26 125(2) . . ? F24A P20 F26 136(2) . . ? F25A P20 F23A 83(2) . . ? F24A P20 F23A 166.2(19) . . ? F26 P20 F23A 42.6(15) . . ? F25A P20 F24 140(2) . . ? F24A P20 F24 46.5(19) . . ? F26 P20 F24 93.1(5) . . ? F23A P20 F24 135.7(17) . . ? F25A P20 F22 80.1(19) . . ? F24A P20 F22 102.7(15) . . ? F26 P20 F22 90.3(3) . . ? F23A P20 F22 91.1(12) . . ? F24 P20 F22 87.6(3) . . ? F25A P20 F21 99.5(18) . . ? F24A P20 F21 76.6(15) . . ? F26 P20 F21 90.6(3) . . ? F23A P20 F21 89.6(12) . . ? F24 P20 F21 92.2(3) . . ? F22 P20 F21 179.1(3) . . ? F25A P20 F23 36(2) . . ? F24A P20 F23 129(2) . . ? F26 P20 F23 91.6(4) . . ? F23A P20 F23 48.9(15) . . ? F24 P20 F23 175.3(5) . . ? F22 P20 F23 92.0(3) . . ? F21 P20 F23 88.1(3) . . ? F25A P20 F25 54(2) . . ? F24A P20 F25 45.6(19) . . ? F26 P20 F25 178.6(5) . . ? F23A P20 F25 136.0(16) . . ? F24 P20 F25 88.3(4) . . ? F22 P20 F25 89.4(3) . . ? F21 P20 F25 89.7(3) . . ? F23 P20 F25 87.1(4) . . ? F25A P20 F26A 175(2) . . ? F24A P20 F26A 85(2) . . ? F26 P20 F26A 51.1(13) . . ? F23A P20 F26A 93(2) . . ? F24 P20 F26A 42.9(13) . . ? F22 P20 F26A 95.9(10) . . ? F21 P20 F26A 84.6(10) . . ? F23 P20 F26A 141.7(14) . . ? F25 P20 F26A 130.3(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C209 H20G O11 0.95 2.51 3.383(9) 152.1 . C206 H20D O11 0.95 2.69 3.525(9) 146.4 . C117 H11G F25 0.95 2.65 3.422(9) 138.7 . C117 H11G F24A 0.95 2.55 3.24(4) 129.9 . C131 H13E F22 0.95 2.62 3.444(7) 145.1 . O241 H24G O21 0.95(7) 1.69(7) 2.619(7) 165(6) 1_565 O201 H20A F14 0.84 2.26 3.090(7) 168.7 4_576 O201 H20A F15 0.84 2.60 3.254(7) 135.5 4_576 O201 H20A F12 0.84 2.63 3.202(6) 126.8 4_576 O141 H14C F16 0.84 2.16 2.985(6) 166.1 1_565 O101 H10A O241 0.93(7) 1.81(7) 2.718(6) 164(6) 4_686 C123 H12F F26 0.95 2.82 3.675(9) 150.6 2_455 C133 H13F O11 0.95 2.56 3.486(8) 165.2 2_455 C139 H13I F15 0.95 2.51 3.229(7) 133.0 1_465 C106 H10D F13 0.95 2.62 3.492(8) 152.8 2_565 C106 H10D F16 0.95 2.63 3.072(8) 109.1 2_565 C207 H20E O101 0.95 2.75 3.355(8) 121.9 3_576 C208 H20F O101 0.95 2.68 3.321(8) 125.3 3_576 C231 H23E F21 0.95 2.70 3.638(8) 169.9 2_445 C231 H23E F25 0.95 2.81 3.441(8) 124.5 2_445 C217 H21G F26 0.95 2.59 3.459(9) 152.5 1_655 C217 H21G F23A 0.95 2.65 3.40(4) 135.6 1_655 C233 H23F O11 0.95 2.69 3.552(8) 151.0 2 O141 H14C O141 0.84 2.57 2.880(9) 102.9 3_575 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.439 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.087 data_al6 _database_code_CSD 211777 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H86 Cl2 Cu2 N8 O4' _chemical_formula_weight 1373.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 15.355(5) _cell_length_b 16.454(5) _cell_length_c 16.555(5) _cell_angle_alpha 115.860(7) _cell_angle_beta 95.746(9) _cell_angle_gamma 110.080(7) _cell_volume 3377.0(19) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2904 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 13613 _diffrn_reflns_av_R_equivalents 0.1500 _diffrn_reflns_av_sigmaI/netI 0.3582 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8575 _reflns_number_gt 2790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1969P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8575 _refine_ls_number_parameters 470 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.2953 _refine_ls_R_factor_gt 0.1391 _refine_ls_wR_factor_ref 0.4035 _refine_ls_wR_factor_gt 0.3213 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 1.0108(4) 0.7542(4) 0.9099(4) 0.0535(16) Uani 1 1 d . . . Cl2 Cl 1.2660(4) 0.1728(4) 0.6868(4) 0.0546(17) Uani 1 1 d . . . Cu1 Cu 1.88922(18) 0.26013(16) 1.70191(17) 0.0399(8) Uani 1 1 d U . . Cu2 Cu 1.42947(17) 0.28692(16) 1.14080(17) 0.0363(8) Uani 1 1 d U . . O101 O 1.8332(10) 0.1391(11) 1.9053(9) 0.065(5) Uani 1 1 d . . . H10G H 1.8452 0.1865 1.9596 0.097 Uiso 1 1 calc R . . C102 C 1.8759(14) 0.1769(13) 1.8522(12) 0.035(2) Uani 1 1 d . . . H10A H 1.9468 0.2147 1.8829 0.042 Uiso 1 1 calc R . . H10B H 1.8509 0.2242 1.8502 0.042 Uiso 1 1 calc R . . C103 C 1.8573(14) 0.0988(13) 1.7561(13) 0.035(2) Uani 1 1 d . . . N104 N 1.8616(11) 0.1250(10) 1.6898(11) 0.035(2) Uani 1 1 d . . . C105 C 1.8497(14) 0.0590(13) 1.6023(14) 0.035(2) Uani 1 1 d . . . C106 C 1.8263(13) -0.0435(13) 1.5728(13) 0.035(2) Uani 1 1 d . . . H10C H 1.8148 -0.0917 1.5095 0.042 Uiso 1 1 calc R . . C107 C 1.8215(14) -0.0675(14) 1.6430(14) 0.0422(16) Uani 1 1 d . . . H10D H 1.8068 -0.1347 1.6267 0.051 Uiso 1 1 calc R . . C108 C 1.8363(14) -0.0017(13) 1.7323(14) 0.038(3) Uani 1 1 d . . . H10E H 1.8330 -0.0212 1.7786 0.045 Uiso 1 1 calc R . . C109 C 1.8601(12) 0.0928(14) 1.5352(12) 0.030(5) Uani 1 1 d . . . H10F H 1.8502 0.0481 1.4709 0.036 Uiso 1 1 calc R . . N110 N 1.8836(11) 0.1871(11) 1.5669(11) 0.0422(16) Uani 1 1 d . . . C111 C 1.8835(15) 0.2150(14) 1.4921(13) 0.041(6) Uani 1 1 d . . . C112 C 1.8025(16) 0.1836(14) 1.4254(15) 0.0422(16) Uani 1 1 d . . . C113 C 1.8096(15) 0.2190(13) 1.3634(14) 0.0422(16) Uani 1 1 d . . . H11A H 1.7536 0.1959 1.3148 0.051 Uiso 1 1 calc R . . C114 C 1.8984(15) 0.2884(13) 1.3717(13) 0.034(5) Uani 1 1 d . . . C115 C 1.9770(16) 0.3220(14) 1.4425(14) 0.0422(16) Uani 1 1 d . . . H11B H 2.0371 0.3706 1.4489 0.051 Uiso 1 1 calc R . . C116 C 1.9729(15) 0.2889(14) 1.5042(14) 0.0422(16) Uani 1 1 d . . . C117 C 2.0609(14) 0.3232(13) 1.5809(14) 0.0422(16) Uani 1 1 d . . . H11C H 2.0401 0.3218 1.6351 0.051 Uiso 1 1 calc R . . H11D H 2.1048 0.3935 1.6018 0.051 Uiso 1 1 calc R . . C118 C 2.1176(14) 0.2593(13) 1.5511(14) 0.0422(16) Uani 1 1 d . . . H11E H 2.1838 0.2975 1.5940 0.063 Uiso 1 1 calc R . . H11F H 2.1199 0.2416 1.4869 0.063 Uiso 1 1 calc R . . H11G H 2.0852 0.1980 1.5535 0.063 Uiso 1 1 calc R . . C119 C 1.697(2) 0.087(2) 1.3975(18) 0.096(10) Uani 1 1 d . . . H11H H 1.6532 0.0637 1.3361 0.115 Uiso 1 1 calc R . . H11I H 1.7074 0.0301 1.3960 0.115 Uiso 1 1 calc R . . C120 C 1.6609(16) 0.1298(15) 1.4716(15) 0.055(4) Uani 1 1 d . . . H12C H 1.5983 0.0796 1.4637 0.082 Uiso 1 1 calc R . . H12D H 1.6524 0.1862 1.4716 0.082 Uiso 1 1 calc R . . H12E H 1.7069 0.1538 1.5313 0.082 Uiso 1 1 calc R . . C121 C 1.9029(16) 0.3244(16) 1.3003(15) 0.055(4) Uani 1 1 d . . . H12A H 1.9124 0.2759 1.2442 0.066 Uiso 1 1 calc R . . H12B H 1.9608 0.3894 1.3282 0.066 Uiso 1 1 calc R . . C122 C 1.8140(16) 0.3378(16) 1.2679(17) 0.055(4) Uani 1 1 d . . . C123 C 1.7876(14) 0.4011(13) 1.3336(14) 0.038(3) Uani 1 1 d . . . H12F H 1.8225 0.4357 1.3983 0.045 Uiso 1 1 calc R . . C124 C 1.7040(15) 0.4151(13) 1.3027(14) 0.038(3) Uani 1 1 d . . . C125 C 1.6576(15) 0.3643(14) 1.2119(15) 0.0422(16) Uani 1 1 d . . . C126 C 1.6844(15) 0.3010(14) 1.1446(14) 0.0422(16) Uani 1 1 d . . . C127 C 1.7680(14) 0.2892(14) 1.1734(15) 0.0422(16) Uani 1 1 d . . . H12G H 1.7911 0.2489 1.1285 0.051 Uiso 1 1 calc R . . C128 C 1.6311(14) 0.2444(13) 1.0399(13) 0.0422(16) Uani 1 1 d . . . H12H H 1.5772 0.2629 1.0320 0.051 Uiso 1 1 calc R . . H12L H 1.6765 0.2686 1.0084 0.051 Uiso 1 1 calc R . . C129 C 1.5905(15) 0.1341(13) 0.9898(14) 0.051(3) Uani 1 1 d . . . H12I H 1.5344 0.1059 0.9361 0.076 Uiso 1 1 calc R . . H12J H 1.5700 0.1101 1.0326 0.076 Uiso 1 1 calc R . . H12K H 1.6401 0.1131 0.9675 0.076 Uiso 1 1 calc R . . C130 C 1.6768(13) 0.4814(13) 1.3783(13) 0.0358(19) Uani 1 1 d . . . H13A H 1.7333 0.5240 1.4355 0.043 Uiso 1 1 calc R . . H13I H 1.6623 0.5261 1.3598 0.043 Uiso 1 1 calc R . . C131 C 1.5952(14) 0.4316(13) 1.4013(13) 0.044(3) Uani 1 1 d . . . H13B H 1.5926 0.4793 1.4616 0.066 Uiso 1 1 calc R . . H13C H 1.6017 0.3764 1.4058 0.066 Uiso 1 1 calc R . . H13D H 1.5354 0.4050 1.3522 0.066 Uiso 1 1 calc R . . N132 N 1.5707(11) 0.3759(10) 1.1797(11) 0.0358(19) Uani 1 1 d . . . C133 C 1.5891(14) 0.4615(13) 1.1821(13) 0.0358(19) Uani 1 1 d . . . H13E H 1.6537 0.5100 1.1994 0.043 Uiso 1 1 calc R . . C134 C 1.5075(14) 0.4780(14) 1.1575(13) 0.0358(19) Uani 1 1 d . . . N135 N 1.4177(11) 0.4083(10) 1.1371(10) 0.032(4) Uani 1 1 d . . . C136 C 1.3380(15) 0.4172(13) 1.1090(14) 0.0358(19) Uani 1 1 d . . . C137 C 1.3485(14) 0.5031(13) 1.1020(13) 0.0358(19) Uani 1 1 d . . . H13F H 1.2931 0.5111 1.0829 0.043 Uiso 1 1 calc R . . C138 C 1.4401(14) 0.5738(13) 1.1233(13) 0.0358(19) Uani 1 1 d . . . H13G H 1.4477 0.6307 1.1176 0.043 Uiso 1 1 calc R . . C139 C 1.5205(15) 0.5645(14) 1.1525(14) 0.048(6) Uani 1 1 d . . . H13H H 1.5837 0.6151 1.1691 0.058 Uiso 1 1 calc R . . C140 C 1.2435(14) 0.3419(14) 1.0876(14) 0.042(6) Uani 1 1 d . . . H14A H 1.2377 0.2766 1.0385 0.050 Uiso 1 1 calc R . . H14B H 1.2375 0.3371 1.1445 0.050 Uiso 1 1 calc R . . O141 O 1.1687(10) 0.3576(10) 1.0576(10) 0.056(4) Uani 1 1 d . . . H14C H 1.1159 0.3103 1.0463 0.084 Uiso 1 1 calc R . . O201 O 2.2207(10) 0.3515(9) 1.8065(11) 0.067(5) Uani 1 1 d . . . H20G H 2.2351 0.3030 1.7822 0.100 Uiso 1 1 calc R . . C202 C 2.1220(16) 0.3158(14) 1.7974(15) 0.051(3) Uani 1 1 d . . . H20A H 2.1060 0.2758 1.8289 0.061 Uiso 1 1 calc R . . H20B H 2.0848 0.2712 1.7300 0.061 Uiso 1 1 calc R . . C203 C 2.0922(17) 0.4003(15) 1.8399(15) 0.051(3) Uani 1 1 d . . . N204 N 2.0029(13) 0.3863(11) 1.8107(12) 0.051(3) Uani 1 1 d . . . C205 C 1.9769(16) 0.4585(14) 1.8539(15) 0.051(3) Uani 1 1 d . . . C206 C 2.0437(17) 0.5527(14) 1.9261(15) 0.051(3) Uani 1 1 d . . . H20C H 2.0234 0.6042 1.9552 0.061 Uiso 1 1 calc R . . C207 C 2.1365(17) 0.5713(15) 1.9547(15) 0.063(7) Uani 1 1 d . . . H20D H 2.1835 0.6356 2.0030 0.075 Uiso 1 1 calc R . . C208 C 2.1607(18) 0.4938(16) 1.9114(16) 0.064(7) Uani 1 1 d . . . H20E H 2.2257 0.5040 1.9307 0.077 Uiso 1 1 calc R . . C209 C 1.8743(15) 0.4377(15) 1.8185(14) 0.0409(19) Uani 1 1 d . . . H20F H 1.8513 0.4870 1.8473 0.049 Uiso 1 1 calc R . . N210 N 1.8160(12) 0.3484(12) 1.7458(11) 0.0409(19) Uani 1 1 d . . . C211 C 1.7224(15) 0.3348(15) 1.7068(14) 0.0409(19) Uani 1 1 d . . . C212 C 1.7083(15) 0.3909(15) 1.6684(14) 0.0409(19) Uani 1 1 d . . . C213 C 1.6181(14) 0.3748(14) 1.6257(13) 0.0409(19) Uani 1 1 d . . . H21A H 1.6109 0.4144 1.6000 0.049 Uiso 1 1 calc R . . C214 C 1.5373(15) 0.2987(15) 1.6210(14) 0.0409(19) Uani 1 1 d . . . C215 C 1.5501(17) 0.2420(16) 1.6601(14) 0.052(6) Uani 1 1 d . . . H21B H 1.4952 0.1929 1.6606 0.062 Uiso 1 1 calc R . . C216 C 1.6398(16) 0.2570(15) 1.6969(13) 0.0409(19) Uani 1 1 d D . . C217 C 1.6438(15) 0.1695(15) 1.7234(13) 0.0409(19) Uani 1 1 d . . . H21C H 1.5832 0.1066 1.6879 0.049 Uiso 1 1 calc R . . H21D H 1.6997 0.1546 1.7100 0.049 Uiso 1 1 calc R . . C218 C 1.6534(15) 0.2122(14) 1.8124(12) 0.045(2) Uani 1 1 d D . . H21E H 1.6571 0.1676 1.8356 0.067 Uiso 1 1 calc R . . H21F H 1.5975 0.2266 1.8236 0.067 Uiso 1 1 calc R . . H21I H 1.7130 0.2750 1.8456 0.067 Uiso 1 1 calc R . . C219 C 1.7967(17) 0.4685(15) 1.6626(17) 0.073(8) Uani 1 1 d . . . H21G H 1.7775 0.5191 1.6599 0.088 Uiso 1 1 calc R . . H21H H 1.8496 0.5035 1.7218 0.088 Uiso 1 1 calc R . . C220 C 1.8356(15) 0.4317(14) 1.5854(14) 0.048(3) Uani 1 1 d . . . H22C H 1.8791 0.4881 1.5807 0.073 Uiso 1 1 calc R . . H22D H 1.7823 0.3852 1.5268 0.073 Uiso 1 1 calc R . . H22E H 1.8718 0.3968 1.5963 0.073 Uiso 1 1 calc R . . C221 C 1.4349(14) 0.2804(13) 1.5762(12) 0.035(3) Uani 1 1 d . . . H22A H 1.3866 0.2239 1.5786 0.042 Uiso 1 1 calc R . . H22B H 1.4248 0.3407 1.6136 0.042 Uiso 1 1 calc R . . C222 C 1.4177(15) 0.2575(14) 1.4779(14) 0.044(3) Uani 1 1 d . . . C223 C 1.3805(15) 0.3094(14) 1.4484(15) 0.048(3) Uani 1 1 d . . . H22F H 1.3690 0.3620 1.4932 0.058 Uiso 1 1 calc R . . C224 C 1.3595(15) 0.2862(14) 1.3547(15) 0.045(2) Uani 1 1 d . . . C225 C 1.3806(15) 0.2150(14) 1.2869(15) 0.045(2) Uani 1 1 d . . . C226 C 1.4281(15) 0.1623(14) 1.3155(15) 0.045(2) Uani 1 1 d . . . C227 C 1.4441(14) 0.1873(13) 1.4108(14) 0.045(2) Uani 1 1 d . . . H22G H 1.4743 0.1552 1.4312 0.054 Uiso 1 1 calc R . . C228 C 1.4618(15) 0.0917(14) 1.2497(14) 0.045(2) Uani 1 1 d . . . H22H H 1.4783 0.0551 1.2783 0.054 Uiso 1 1 calc R . . H22I H 1.4080 0.0419 1.1909 0.054 Uiso 1 1 calc R . . C229 C 1.5472(15) 0.1425(14) 1.2266(14) 0.048(3) Uani 1 1 d . . . H22J H 1.5703 0.0937 1.1888 0.073 Uiso 1 1 calc R . . H22K H 1.5990 0.1957 1.2848 0.073 Uiso 1 1 calc R . . H22L H 1.5290 0.1715 1.1909 0.073 Uiso 1 1 calc R . . C230 C 1.3108(16) 0.3366(14) 1.3237(14) 0.048(3) Uani 1 1 d . . . H23A H 1.3273 0.4036 1.3776 0.058 Uiso 1 1 calc R . . H23B H 1.3361 0.3464 1.2744 0.058 Uiso 1 1 calc R . . C231 C 1.2036(15) 0.2790(15) 1.2866(15) 0.055(6) Uani 1 1 d . . . H23C H 1.1764 0.3095 1.2579 0.082 Uiso 1 1 calc R . . H23D H 1.1768 0.2799 1.3381 0.082 Uiso 1 1 calc R . . H23E H 1.1867 0.2097 1.2392 0.082 Uiso 1 1 calc R . . N232 N 1.3690(13) 0.1961(12) 1.1957(12) 0.048(3) Uani 1 1 d . . . C233 C 1.3125(15) 0.1079(14) 1.1288(14) 0.044(3) Uani 1 1 d . . . H23F H 1.2777 0.0585 1.1434 0.053 Uiso 1 1 calc R . . C234 C 1.3000(14) 0.0812(13) 1.0321(13) 0.035(3) Uani 1 1 d . . . N235 N 1.3486(11) 0.1556(10) 1.0155(10) 0.035(3) Uani 1 1 d . . . C236 C 1.3403(14) 0.1348(13) 0.9272(13) 0.035(3) Uani 1 1 d . . . C237 C 1.2855(14) 0.0427(12) 0.8524(13) 0.041(3) Uani 1 1 d . . . H23G H 1.2827 0.0306 0.7904 0.049 Uiso 1 1 calc R . . C238 C 1.2332(15) -0.0346(13) 0.8675(13) 0.041(3) Uani 1 1 d . . . H23H H 1.1950 -0.1003 0.8158 0.049 Uiso 1 1 calc R . . C239 C 1.2370(15) -0.0152(13) 0.9560(13) 0.041(3) Uani 1 1 d . . . H23I H 1.1979 -0.0659 0.9672 0.049 Uiso 1 1 calc R . . C240 C 1.3916(15) 0.2220(12) 0.9116(13) 0.041(3) Uani 1 1 d . . . H24A H 1.3466 0.2515 0.9057 0.049 Uiso 1 1 calc R . . H24B H 1.4482 0.2744 0.9672 0.049 Uiso 1 1 calc R . . O241 O 1.4229(10) 0.1936(9) 0.8319(9) 0.048(4) Uani 1 1 d . . . H24C H 1.3831 0.1859 0.7875 0.072 Uiso 1 1 calc R . . C01 C 0.0525(12) -0.0437(13) 0.7203(9) 0.083(8) Uiso 1 1 d G . . H01A H 0.0542 -0.0772 0.6574 0.100 Uiso 1 1 calc R . . C02 C 0.0868(11) 0.0598(13) 0.7690(12) 0.081(8) Uiso 1 1 d G . . H02A H 0.1120 0.0971 0.7394 0.097 Uiso 1 1 calc R . . C03 C 0.0843(12) 0.1089(9) 0.8610(11) 0.069(7) Uiso 1 1 d G . . H03A H 0.1078 0.1797 0.8943 0.083 Uiso 1 1 calc R . . C04 C 0.0475(13) 0.0543(13) 0.9043(9) 0.109(10) Uiso 1 1 d G . . H04A H 0.0458 0.0878 0.9671 0.130 Uiso 1 1 calc R . . C05 C 0.0132(12) -0.0493(13) 0.8555(12) 0.084(8) Uiso 1 1 d G . . H05A H -0.0120 -0.0866 0.8851 0.101 Uiso 1 1 calc R . . C06 C 0.0157(12) -0.0983(9) 0.7636(12) 0.090(9) Uiso 1 1 d G . . H06A H -0.0078 -0.1691 0.7303 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 Cl1 0.086(5) 0.047(3) 0.075(4) 0.048(3) 0.047(3) 0.049(3) Cl2 0.086(5) 0.042(3) 0.072(4) 0.042(3) 0.035(3) 0.045(3) Cu1 0.0608(16) 0.0201(12) 0.0574(16) 0.0254(11) 0.0209(12) 0.0282(11) Cu2 0.0515(14) 0.0160(11) 0.0518(14) 0.0244(10) 0.0113(10) 0.0171(9) O101 0.086(12) 0.078(12) 0.055(10) 0.052(9) 0.045(9) 0.032(9) C102 0.055(6) 0.021(5) 0.047(6) 0.026(4) 0.017(5) 0.023(4) C103 0.055(6) 0.021(5) 0.047(6) 0.026(4) 0.017(5) 0.023(4) N104 0.055(6) 0.021(5) 0.047(6) 0.026(4) 0.017(5) 0.023(4) C105 0.055(6) 0.021(5) 0.047(6) 0.026(4) 0.017(5) 0.023(4) C106 0.055(6) 0.021(5) 0.047(6) 0.026(4) 0.017(5) 0.023(4) C107 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C108 0.063(9) 0.019(6) 0.050(8) 0.026(6) 0.023(7) 0.024(6) C109 0.037(12) 0.039(12) 0.014(10) 0.008(10) 0.015(9) 0.021(10) N110 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C111 0.077(17) 0.037(13) 0.031(12) 0.030(11) 0.024(11) 0.029(12) C112 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C113 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C114 0.061(15) 0.028(11) 0.033(12) 0.023(10) 0.023(11) 0.027(11) C115 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C116 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C117 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C118 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C119 0.20(3) 0.12(2) 0.078(19) 0.082(19) 0.08(2) 0.13(2) C120 0.075(10) 0.041(8) 0.086(10) 0.049(8) 0.032(8) 0.042(7) C121 0.075(10) 0.041(8) 0.086(10) 0.049(8) 0.032(8) 0.042(7) C122 0.075(10) 0.041(8) 0.086(10) 0.049(8) 0.032(8) 0.042(7) C123 0.063(9) 0.019(6) 0.050(8) 0.026(6) 0.023(7) 0.024(6) C124 0.063(9) 0.019(6) 0.050(8) 0.026(6) 0.023(7) 0.024(6) C125 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C126 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C127 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C128 0.060(4) 0.023(3) 0.060(4) 0.033(3) 0.018(3) 0.019(3) C129 0.073(7) 0.025(5) 0.067(6) 0.026(5) 0.015(5) 0.033(5) C130 0.049(5) 0.025(4) 0.058(5) 0.032(4) 0.021(4) 0.027(4) C131 0.068(9) 0.020(7) 0.047(8) 0.009(6) 0.031(7) 0.028(6) N132 0.049(5) 0.025(4) 0.058(5) 0.032(4) 0.021(4) 0.027(4) C133 0.049(5) 0.025(4) 0.058(5) 0.032(4) 0.021(4) 0.027(4) C134 0.049(5) 0.025(4) 0.058(5) 0.032(4) 0.021(4) 0.027(4) N135 0.038(10) 0.011(8) 0.047(10) 0.019(8) 0.017(8) 0.006(7) C136 0.049(5) 0.025(4) 0.058(5) 0.032(4) 0.021(4) 0.027(4) C137 0.049(5) 0.025(4) 0.058(5) 0.032(4) 0.021(4) 0.027(4) C138 0.049(5) 0.025(4) 0.058(5) 0.032(4) 0.021(4) 0.027(4) C139 0.048(15) 0.016(11) 0.063(15) 0.014(11) 0.005(11) 0.005(10) C140 0.046(15) 0.037(13) 0.063(15) 0.042(12) 0.018(11) 0.018(11) O141 0.040(10) 0.040(9) 0.100(12) 0.044(9) 0.013(8) 0.020(7) O201 0.065(11) 0.026(8) 0.118(14) 0.029(9) 0.039(10) 0.036(8) C202 0.073(7) 0.025(5) 0.067(6) 0.026(5) 0.015(5) 0.033(5) C203 0.073(7) 0.025(5) 0.067(6) 0.026(5) 0.015(5) 0.033(5) N204 0.073(7) 0.025(5) 0.067(6) 0.026(5) 0.015(5) 0.033(5) C205 0.073(7) 0.025(5) 0.067(6) 0.026(5) 0.015(5) 0.033(5) C206 0.073(7) 0.025(5) 0.067(6) 0.026(5) 0.015(5) 0.033(5) C207 0.055(17) 0.029(13) 0.067(17) 0.001(12) -0.019(13) 0.021(12) C208 0.09(2) 0.044(15) 0.078(18) 0.038(14) 0.011(15) 0.047(15) C209 0.061(6) 0.046(5) 0.054(5) 0.037(4) 0.037(4) 0.041(4) N210 0.061(6) 0.046(5) 0.054(5) 0.037(4) 0.037(4) 0.041(4) C211 0.061(6) 0.046(5) 0.054(5) 0.037(4) 0.037(4) 0.041(4) C212 0.061(6) 0.046(5) 0.054(5) 0.037(4) 0.037(4) 0.041(4) C213 0.061(6) 0.046(5) 0.054(5) 0.037(4) 0.037(4) 0.041(4) C214 0.061(6) 0.046(5) 0.054(5) 0.037(4) 0.037(4) 0.041(4) C215 0.070(17) 0.065(16) 0.065(16) 0.047(14) 0.033(13) 0.054(14) C216 0.061(6) 0.046(5) 0.054(5) 0.037(4) 0.037(4) 0.041(4) C217 0.061(6) 0.046(5) 0.054(5) 0.037(4) 0.037(4) 0.041(4) C218 0.067(6) 0.030(5) 0.062(6) 0.029(5) 0.032(5) 0.036(4) C219 0.09(2) 0.028(13) 0.082(19) 0.027(14) 0.011(15) 0.009(13) C220 0.078(7) 0.024(5) 0.057(6) 0.022(5) 0.027(5) 0.033(5) C221 0.072(7) 0.013(5) 0.041(6) 0.019(5) 0.034(6) 0.028(5) C222 0.068(9) 0.020(7) 0.047(8) 0.009(6) 0.031(7) 0.028(6) C223 0.078(7) 0.024(5) 0.057(6) 0.022(5) 0.027(5) 0.033(5) C224 0.067(6) 0.030(5) 0.062(6) 0.029(5) 0.032(5) 0.036(4) C225 0.067(6) 0.030(5) 0.062(6) 0.029(5) 0.032(5) 0.036(4) C226 0.067(6) 0.030(5) 0.062(6) 0.029(5) 0.032(5) 0.036(4) C227 0.067(6) 0.030(5) 0.062(6) 0.029(5) 0.032(5) 0.036(4) C228 0.067(6) 0.030(5) 0.062(6) 0.029(5) 0.032(5) 0.036(4) C229 0.078(7) 0.024(5) 0.057(6) 0.022(5) 0.027(5) 0.033(5) C230 0.078(7) 0.024(5) 0.057(6) 0.022(5) 0.027(5) 0.033(5) C231 0.083(19) 0.043(14) 0.070(16) 0.036(13) 0.028(14) 0.050(14) N232 0.078(7) 0.024(5) 0.057(6) 0.022(5) 0.027(5) 0.033(5) C233 0.068(9) 0.020(7) 0.047(8) 0.009(6) 0.031(7) 0.028(6) C234 0.072(7) 0.013(5) 0.041(6) 0.019(5) 0.034(6) 0.028(5) N235 0.072(7) 0.013(5) 0.041(6) 0.019(5) 0.034(6) 0.028(5) C236 0.072(7) 0.013(5) 0.041(6) 0.019(5) 0.034(6) 0.028(5) C237 0.076(8) 0.010(5) 0.041(6) 0.018(5) 0.018(6) 0.017(5) C238 0.076(8) 0.010(5) 0.041(6) 0.018(5) 0.018(6) 0.017(5) C239 0.076(8) 0.010(5) 0.041(6) 0.018(5) 0.018(6) 0.017(5) C240 0.076(8) 0.010(5) 0.041(6) 0.018(5) 0.018(6) 0.017(5) O241 0.074(11) 0.042(9) 0.055(9) 0.037(8) 0.034(8) 0.034(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 Cu1 N110 1.999(16) . ? Cu1 N104 2.027(14) . ? Cu1 N204 2.055(17) . ? Cu1 N210 2.065(16) . ? Cu2 N132 1.994(15) . ? Cu2 N235 2.061(15) . ? Cu2 N232 2.079(17) . ? Cu2 N135 2.092(15) . ? O101 C102 1.379(19) . ? C102 C103 1.46(2) . ? C103 N104 1.34(2) . ? C103 C108 1.43(2) . ? N104 C105 1.32(2) . ? C105 C106 1.43(2) . ? C105 C109 1.44(2) . ? C106 C107 1.38(2) . ? C107 C108 1.33(2) . ? C109 N110 1.30(2) . ? N110 C111 1.50(2) . ? C111 C112 1.35(3) . ? C111 C116 1.41(3) . ? C112 C113 1.38(2) . ? C112 C119 1.68(3) . ? C113 C114 1.39(2) . ? C114 C115 1.35(2) . ? C114 C121 1.53(2) . ? C115 C116 1.35(2) . ? C116 C117 1.50(3) . ? C117 C118 1.54(3) . ? C119 C120 1.40(3) . ? C121 C122 1.54(3) . ? C122 C123 1.35(3) . ? C122 C127 1.37(3) . ? C123 C124 1.46(3) . ? C124 C125 1.32(2) . ? C124 C130 1.47(2) . ? C125 C126 1.37(3) . ? C125 N132 1.49(2) . ? C126 C127 1.43(3) . ? C126 C128 1.52(3) . ? C128 C129 1.47(2) . ? C130 C131 1.43(2) . ? N132 C133 1.32(2) . ? C133 C134 1.43(3) . ? C134 N135 1.35(2) . ? C134 C139 1.41(3) . ? N135 C136 1.34(2) . ? C136 C137 1.42(2) . ? C136 C140 1.43(2) . ? C137 C138 1.37(2) . ? C138 C139 1.36(3) . ? C140 O141 1.35(2) . ? O201 C202 1.39(2) . ? C202 C203 1.51(3) . ? C203 N204 1.31(2) . ? C203 C208 1.39(3) . ? N204 C205 1.31(2) . ? C205 C206 1.39(3) . ? C205 C209 1.49(3) . ? C206 C207 1.34(3) . ? C207 C208 1.36(3) . ? C209 N210 1.32(2) . ? N210 C211 1.41(2) . ? C211 C212 1.39(3) . ? C211 C216 1.39(3) . ? C212 C213 1.37(3) . ? C212 C219 1.56(3) . ? C213 C214 1.39(3) . ? C214 C215 1.40(3) . ? C214 C221 1.54(3) . ? C215 C216 1.34(3) . ? C216 C217 1.70(2) . ? C217 C218 1.29(2) . ? C219 C220 1.44(3) . ? C221 C222 1.47(2) . ? C222 C223 1.39(3) . ? C222 C227 1.42(3) . ? C223 C224 1.40(3) . ? C224 C225 1.39(3) . ? C224 C230 1.49(3) . ? C225 N232 1.38(2) . ? C225 C226 1.49(3) . ? C226 C227 1.42(3) . ? C226 C228 1.49(3) . ? C228 C229 1.48(2) . ? C230 C231 1.48(3) . ? N232 C233 1.28(2) . ? C233 C234 1.44(2) . ? C234 N235 1.36(2) . ? C234 C239 1.41(2) . ? N235 C236 1.33(2) . ? C236 C237 1.35(2) . ? C236 C240 1.53(2) . ? C237 C238 1.39(2) . ? C238 C239 1.35(2) . ? C240 O241 1.39(2) . ? C01 C02 1.3900 . ? C01 C06 1.3900 . ? C02 C03 1.3900 . ? C03 C04 1.3900 . ? C04 C05 1.3900 . ? C05 C06 1.3900 . ? 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 N110 Cu1 N104 82.3(6) . . ? N110 Cu1 N204 127.7(7) . . ? N104 Cu1 N204 119.4(6) . . ? N110 Cu1 N210 121.2(7) . . ? N104 Cu1 N210 130.2(6) . . ? N204 Cu1 N210 82.3(7) . . ? N132 Cu2 N235 127.4(6) . . ? N132 Cu2 N232 124.3(7) . . ? N235 Cu2 N232 82.0(6) . . ? N132 Cu2 N135 81.7(6) . . ? N235 Cu2 N135 110.9(6) . . ? N232 Cu2 N135 136.4(6) . . ? O101 C102 C103 112.8(15) . . ? N104 C103 C108 120.3(17) . . ? N104 C103 C102 117.5(16) . . ? C108 C103 C102 122.1(17) . . ? C105 N104 C103 120.5(16) . . ? C105 N104 Cu1 110.1(12) . . ? C103 N104 Cu1 129.3(13) . . ? N104 C105 C106 122.2(17) . . ? N104 C105 C109 118.0(16) . . ? C106 C105 C109 119.7(18) . . ? C107 C106 C105 115.3(18) . . ? C108 C107 C106 123.7(18) . . ? C107 C108 C103 117.8(18) . . ? N110 C109 C105 116.7(16) . . ? C109 N110 C111 113.8(16) . . ? C109 N110 Cu1 112.7(12) . . ? C111 N110 Cu1 132.4(12) . . ? C112 C111 C116 121.2(18) . . ? C112 C111 N110 123.6(18) . . ? C116 C111 N110 114.6(17) . . ? C111 C112 C113 118.9(19) . . ? C111 C112 C119 124.2(18) . . ? C113 C112 C119 115.7(19) . . ? C112 C113 C114 120(2) . . ? C115 C114 C113 119.0(18) . . ? C115 C114 C121 122.5(18) . . ? C113 C114 C121 118.5(18) . . ? C116 C115 C114 122.2(19) . . ? C115 C116 C111 118.0(19) . . ? C115 C116 C117 122.5(18) . . ? C111 C116 C117 119.4(17) . . ? C116 C117 C118 113.9(17) . . ? C120 C119 C112 101(2) . . ? C114 C121 C122 116.1(17) . . ? C123 C122 C127 123(2) . . ? C123 C122 C121 118(2) . . ? C127 C122 C121 119(2) . . ? C122 C123 C124 118(2) . . ? C125 C124 C123 118.2(19) . . ? C125 C124 C130 126(2) . . ? C123 C124 C130 115.4(18) . . ? C124 C125 C126 124(2) . . ? C124 C125 N132 118.8(19) . . ? C126 C125 N132 117.3(19) . . ? C125 C126 C127 118(2) . . ? C125 C126 C128 123(2) . . ? C127 C126 C128 118.3(19) . . ? C122 C127 C126 118(2) . . ? C129 C128 C126 117.6(16) . . ? C131 C130 C124 115.3(15) . . ? C133 N132 C125 115.3(15) . . ? C133 N132 Cu2 113.9(13) . . ? C125 N132 Cu2 130.7(11) . . ? N132 C133 C134 116.9(17) . . ? N135 C134 C139 120.5(18) . . ? N135 C134 C133 118.9(17) . . ? C139 C134 C133 120.6(18) . . ? C136 N135 C134 121.6(16) . . ? C136 N135 Cu2 129.4(11) . . ? C134 N135 Cu2 108.6(13) . . ? N135 C136 C137 119.3(17) . . ? N135 C136 C140 120.4(17) . . ? C137 C136 C140 120.3(19) . . ? C138 C137 C136 118.8(19) . . ? C139 C138 C137 121.4(18) . . ? C138 C139 C134 118.3(18) . . ? O141 C140 C136 115.1(17) . . ? O201 C202 C203 111.6(17) . . ? N204 C203 C208 120(2) . . ? N204 C203 C202 121.1(19) . . ? C208 C203 C202 119(2) . . ? C203 N204 C205 119.9(19) . . ? C203 N204 Cu1 128.5(14) . . ? C205 N204 Cu1 111.6(16) . . ? N204 C205 C206 121(2) . . ? N204 C205 C209 117.4(19) . . ? C206 C205 C209 121.0(19) . . ? C207 C206 C205 120(2) . . ? C206 C207 C208 117(2) . . ? C207 C208 C203 121(2) . . ? N210 C209 C205 117.9(18) . . ? C209 N210 C211 116.5(17) . . ? C209 N210 Cu1 110.8(14) . . ? C211 N210 Cu1 132.3(13) . . ? C212 C211 C216 117(2) . . ? C212 C211 N210 122.3(18) . . ? C216 C211 N210 120.6(18) . . ? C213 C212 C211 122.9(19) . . ? C213 C212 C219 116.5(19) . . ? C211 C212 C219 120(2) . . ? C212 C213 C214 118.2(19) . . ? C213 C214 C215 120(2) . . ? C213 C214 C221 119.7(18) . . ? C215 C214 C221 120.6(18) . . ? C216 C215 C214 120(2) . . ? C215 C216 C211 122.1(19) . . ? C215 C216 C217 114.5(17) . . ? C211 C216 C217 123.3(19) . . ? C218 C217 C216 102.6(15) . . ? C220 C219 C212 117.8(18) . . ? C222 C221 C214 113.2(16) . . ? C223 C222 C227 116.9(19) . . ? C223 C222 C221 120.7(18) . . ? C227 C222 C221 122(2) . . ? C222 C223 C224 122(2) . . ? C225 C224 C223 122(2) . . ? C225 C224 C230 117(2) . . ? C223 C224 C230 120.4(19) . . ? N232 C225 C224 124(2) . . ? N232 C225 C226 117.1(18) . . ? C224 C225 C226 119(2) . . ? C227 C226 C228 121.6(19) . . ? C227 C226 C225 115.9(18) . . ? C228 C226 C225 122.5(19) . . ? C226 C227 C222 124(2) . . ? C229 C228 C226 113.1(16) . . ? C231 C230 C224 113.0(17) . . ? C233 N232 C225 118.5(18) . . ? C233 N232 Cu2 109.6(14) . . ? C225 N232 Cu2 131.9(13) . . ? N232 C233 C234 121.8(19) . . ? N235 C234 C239 119.9(17) . . ? N235 C234 C233 116.5(16) . . ? C239 C234 C233 123.5(16) . . ? C236 N235 C234 119.0(15) . . ? C236 N235 Cu2 131.0(12) . . ? C234 N235 Cu2 110.0(12) . . ? N235 C236 C237 123.3(16) . . ? N235 C236 C240 117.2(16) . . ? C237 C236 C240 119.4(17) . . ? C236 C237 C238 118.9(18) . . ? C239 C238 C237 119.4(17) . . ? C238 C239 C234 119.3(17) . . ? O241 C240 C236 112.9(14) . . ? C02 C01 C06 120.0 . . ? C01 C02 C03 120.0 . . ? C02 C03 C04 120.0 . . ? C05 C04 C03 120.0 . . ? C04 C05 C06 120.0 . . ? C05 C06 C01 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O241 H24C Cl2 0.84 2.21 3.041(15) 171.0 . C221 H22A Cl2 0.99 2.87 3.720(18) 144.1 1_556 O201 H20G Cl2 0.84 2.28 3.107(14) 167.4 1_656 C106 H10C Cl2 0.95 2.85 3.71(2) 149.8 2_857 C109 H10F Cl2 0.95 3.09 3.886(18) 142.4 2_857 C239 H23I O101 0.95 2.86 3.69(2) 147.8 2_858 C121 H12A Cl1 0.99 2.84 3.70(2) 146.5 2_867 C209 H20F O141 0.95 2.50 3.43(2) 166.8 2_868 O101 H10G Cl1 0.84 2.50 3.023(15) 121.6 2_868 C139 H13H O201 0.95 2.81 3.61(3) 142.1 2_968 C133 H13E O201 0.95 2.48 3.35(2) 153.3 2_968 O141 H14C Cl1 0.84 2.23 2.991(14) 150.6 2_767 _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.151 _refine_diff_density_min -1.752 _refine_diff_density_rms 0.173